Summary of the invention
The object of the present invention is to provide coating type enzyme granulate of a kind of more energy-conserving and environment-protective and preparation method thereof.
A first aspect of the present invention, provides a kind of coating type enzyme granulate, and described coating type enzyme granulate comprises enzyme ball and dressing, and described enzyme ball contains enzyme component and stablizer, described enzyme component be selected from lower group one or more:
Sumizyme MP, alkaline lipase, cellulase, amylase and mannase;
Described stablizer be selected from lower group one or more:
Glucose, carboxymethyl cellulose, polyoxyethylene glycol, SODIUM PHOSPHATE, MONOBASIC, magnesium chloride, sodium-chlor and starch.
In another preference, the component of described dressing is selected from one or more of lower group:
SODIUM PHOSPHATE, MONOBASIC, polyvinyl alcohol, PVP K30, titanium dioxide, magnesium chloride, starch and bright orchid.
In another preference, in described coating type enzyme granulate, the ratio of weight and number of enzyme ball and dressing material is 40-90:5-20.
In another preference, the ratio of weight and number of described enzyme component and described stablizer is 30-55:35-70; Preferably, the ratio of weight and number of described enzyme component and described stablizer is 45:55.
In another preference, described stablizer be selected from lower group one or more:
Glucose 2-5 weight part, carboxymethyl cellulose 2.5-12 weight part, polyoxyethylene glycol PEG-1500 3-7 weight part, SODIUM PHOSPHATE, MONOBASIC 6-15 weight part, magnesium chloride 10-20 weight part, sodium-chlor 0-5 weight part and W-Gum 15-28 weight part.
In another preference, described stablizer be selected from lower group one or more:
Glucose 3.5 weight part, carboxymethyl cellulose 3.2 weight part, polyoxyethylene glycol PEG-1500 5 weight part, SODIUM PHOSPHATE, MONOBASIC 11 weight part, magnesium chloride 14 weight part and W-Gum 18 weight part.
In another preference, the component of described dressing is selected from one or more of lower group:
SODIUM PHOSPHATE, MONOBASIC 6-15 weight part, polyvinyl alcohol PEG-1000 4-8 weight part, PVP K30 15-21 weight part, magnesium chloride 12-20 weight part, starch 10-25 weight part, titanium dioxide 4-9 weight part and bright blue 0.05-0.1 weight part; Preferably, one or more of lower group: SODIUM PHOSPHATE, MONOBASIC 13 weight part, polyvinyl alcohol PEG-1000 5 weight part, PVP K30 18 weight part, magnesium chloride 18 weight part, starch 24. weight part, titanium dioxide 6 weight part, bright blue 0.06 weight part.
A second aspect of the present invention, provides a kind of method preparing coating type enzyme granulate as described in the first aspect of the invention, comprises the steps:
(1) enzyme ball is prepared
After enzyme component and stablizer being mixed in proportion, adopt the wet enzyme ball of wet-method extrusion prilling process preparation;
(2) enzyme ball dry coationg
Prepare coating components in proportion, be dissolved in the water, make the suspension of 4-10%; The wet enzyme ball of preparation is placed in fluidized-bed, is dried to when temperature of charge reaches 45 DEG C-50 DEG C and carries out dressing.
In another preference, in described step (1), comprise step:
(1.1) wet feed is prepared
Enzyme and stablizer are weighed in proportion and be mixed to get enzyme ball material, add water, the weight ratio of enzyme ball material and water is 3-5:1, mixes to obtain wet feed;
(1.2) round as a ball one-tenth ball is extruded
The wet feed that (1.1) make is put in extrusion machine, through being squeezed into cylindrical strip extrudate; Be placed in by extrudate on spheronizator, round as a ball one-tenth wets enzyme ball.
In another preference, in described step (1.2), control extrusion machine extrudate temperature≤80 DEG C; Preferably ,≤70 DEG C; More preferably ,≤60 DEG C; Most preferably ,≤50 DEG C.
In another preference, the diameter controlling described extrudate in described step (1.2) is 0.3-0.6mm.
In another preference, in described step (2) coating process, control fluidized-bed inlet temperature 45 DEG C-75 DEG C, air quantity 60m
3/ h-170m
3/ h, atomizing pressure 1.25bar-2.5bar.
Should be understood that within the scope of the present invention, above-mentioned each technical characteristic of the present invention and can combining mutually between specifically described each technical characteristic in below (eg embodiment), thus form new or preferred technical scheme.As space is limited, tiredly no longer one by one to state at this.
Embodiment
The present inventor, by extensive and deep research, obtains a kind of coating type enzyme granulate prescription, and this prescription is particularly suitable for adopting wet method extruder grain technique to prepare coating type enzyme granulate.Complete the present invention on this basis.
The object of this invention is to provide a kind of washing enzyme granulation preparation, thus solve traditional granulation dust hazard, propose a kind of safe, easy, efficient preparation method.There is provided that a kind of homogeneity is excellent, the coating type detergent enzymes of constant product quality.One aspect of the present invention relates to washings enzyme wet granulation, and including mass percent is 40%-90% enzyme granulate, and mass percent is the dressing material of 5%-20%.
Wherein enzyme granulate can be the lytic enzymes such as Sumizyme MP, alkaline lipase, cellulase, amylase, mannase.Glucose, carboxymethyl cellulose, polyoxyethylene glycol, SODIUM PHOSPHATE, MONOBASIC, magnesium chloride, sodium-chlor, starch form, and coating components is by SODIUM PHOSPHATE, MONOBASIC, polyvinyl alcohol, PVP K30, titanium dioxide, magnesium chloride, starch, bright orchid.
The optimum quality of above-mentioned enzyme ball component is: the 30%-55% such as washing enzyme Sumizyme MP, alkaline lipase, cellulase, amylase, mannase, glucose 2%-5%, carboxymethyl cellulose 2.5%-12%, polyoxyethylene glycol PEG-1500 3%-7%, SODIUM PHOSPHATE, MONOBASIC 6%-15%, magnesium chloride 10%-20%, W-Gum 15%-28%.Wherein enzyme ball optimum quality component is: washing enzyme Sumizyme MP, alkaline lipase, cellulase, amylase, mannase etc. 45%, glucose 3.5%, carboxymethyl cellulose 3.2%, polyoxyethylene glycol PEG-1500 5%, SODIUM PHOSPHATE, MONOBASIC 11%, magnesium chloride 14%, W-Gum 18.3%.
Above-mentioned coating components SODIUM PHOSPHATE, MONOBASIC 6%-15%, polyvinyl alcohol PEG-1000 4%-8%, PVP K30 15%-21%, magnesium chloride 12%-20%, starch 10%-25%, titanium dioxide 4%-9%, bright blue 0.05%-0.1%, above-mentioned coating components optimum proportion is SODIUM PHOSPHATE, MONOBASIC 13%, polyvinyl alcohol PEG-1000 5%, PVP K30 18%, magnesium chloride 18%, starch 24.04%, titanium dioxide 6%, bright blue 0.06%
1, the making step of enzyme ball is as follows:
1.1, the preparation of wet feed enzyme shattered with auxiliary material such as Microcrystalline Cellulose, glucose etc., sieve, after weigh interpolation in proportion and mix; add the aqueous solution as condensing agent or tackiness agent; the mass ratio of material and water controls at 3.5:1; powder is made there is certain plastic moistening uniform material, or wet feed is made wet granular through tablets press.Wet method requires to possess certain moisture-retaining capacity thus increases the plasticity-of mobility and the round as a ball property extruded.
1.2, the plasticity wet feed the first step made of extrusion process or wet grain are put in extrusion machine, and the fashion of extrusion such as to roll by wet feed by the hole of tool certain diameter or sieve through screw propulsion or rolling, wherein hole sizer diameter selects 0.45mm, is squeezed into cylindrical strip extrudate.Extrude bar and answer smooth surface, extrudate often answers extrusion pressure to generate heat, long-term continuous seepage, and fever phenomenon is more obvious.The inventive method selects subcooled forcing machine, for large production continuously of thermo-sensitivity enzyme provides reliable technical guarantee.
1.3, above-mentioned extrudate heap is discharged on the rotation friction plate of spheronizator by round as a ball one-tenth ball process, extrudate is then dispersed into the less right cylinder that length is equivalent to its diameter, due to the effect of frictional force, these plastic cylindrical materials ceaselessly roll onboard, are rolled into spheroidal gradually.Its round as a ball process, round as a ball process can distinguish several different stage according to particle shape.Round as a ball one-tenth ball process is by initial short cylindrical shape particle, and edge friction plate become under rotary rolling gradually without corner angle is circular right cylinder, and then is rolled into dumb-bell shape, ellipse until become spherical completely.Time round as a ball after the right cylinder forming edge rounding, right cylinder bends, reverse, subsequently right cylinder to break the part that formation two is separated, the face that both tool one is round and flat, due to the effect of revolving force and frictional force, above-mentioned planar recess, as same flower formed cave, then edge bag stack be rolled into spherical.
2, enzyme ball dry coationg: the wet enzyme ball of preparation is placed in fluidized-bed, inlet temperature 45 DEG C-75 DEG C is set, air quantity 100m
3/ h-160m
3/ h, be dried to when temperature of charge reaches 45 DEG C-50 DEG C and carry out dressing, wherein the preparation reference principle once of coating liquid: take after coating powder sieves and be dissolved in water, be mixed with 4%-10% suspension and sieve, then condition fluidized-bed inlet temperature 45 DEG C-75 DEG C, air quantity 60m
3/ h-170m
3/ h, atomizing pressure 1.25bar-2.5bar.
Major advantage of the present invention is:
(1) wet-method extrusion granulation process is adopted to prepare coating type enzyme granulate first;
(2) a kind of coating type enzyme granulate prescription being suitable for wet-method extrusion granulation process is provided;
(3) adopt prescription of the present invention and coordinate wet-method extrusion prilling process of the present invention to prepare coating type enzyme granulate, achieve detersive enzyme safe, easy, prepare efficiently, achieve low dust or without dust granulation, improve the stability of production technique, reduce human factor to problems such as the impacts of quality product and yield.
(4) technical scheme provided by the invention, enzyme granulate and washing powder have good mixture homogeneity, enzyme granulate disintegration time is short, the shelf time is long, and the coating type enzyme granulate homogeneity of preparation is good, steady quality.
(5) technical scheme of the present invention more energy-conserving and environment-protective, whole technological operation is easy, extremely low to technical experience requirement.
Detection method
1, enzyme is lived: the detection carrying out enzyme activity according to industrial enzyme preparation GENERAL EXPERIMENTATION (QB/T 1803-1993).
Enzyme storage rate alive:
X=E
1/E×100%
X: the enzyme activity storage rate % of sample
E
1: sample actual measurement enzyme activity (u/g or u/ml)
E: sample marker (before preservation) enzyme activity (u/g or u/ml)
2, solvability: enzyme granulate and water are put into water with 1: 100 ratio, room temperature lower magnetic force stirs low rate mixing, record enzyme granulate disintegration time.
3, weight loss on drying: the detection carrying out weight loss on drying according to industrial enzyme preparation universal test method (QB/T 1803-1993).
4, stability: 37 DEG C, preserve 9 months under 70% humidity condition, detect enzyme and to live storage rate.
5, homogeneity: random sampling 1kg, sieves with standard sieve, detects 30 order ~ 60 order particle accountings.
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.Unless otherwise indicated, otherwise per-cent and number calculate by weight.
Embodiment 1
(1) material prepares
Material is prepared according to following listed parts by weight.
In enzyme ball, the parts by weight of each component are:
Enzyme component: Sumizyme MP 45 weight part;
Stabilizer component: glucose 3.5 weight part, carboxymethyl cellulose 3.2 weight part, polyoxyethylene glycol PEG-1500 5 weight part, SODIUM PHOSPHATE, MONOBASIC 11 weight part, magnesium chloride 14 weight part, W-Gum 18.3 weight part.
In dressing, the parts by weight of each component are:
SODIUM PHOSPHATE, MONOBASIC 13 weight part, polyvinyl alcohol PEG-1000 5 weight part, PVP K30 18 weight part, magnesium chloride 18 weight part, starch 24.04 weight part, titanium dioxide 6 weight part, bright blue 0.06 weight part.
(2) coating type enzyme granulate is prepared
1, the making step of enzyme ball is as follows:
1.1, the preparation of wet feed
Enzyme and stablizer are shattered respectively, sieve after weigh in proportion, mix, add the aqueous solution as condensing agent or tackiness agent, the mass ratio of material and water is 3.5:1, after mixing wet feed.Use above-mentioned enzyme ball formula, wet feed moisture-retaining capacity obtained under this material-water ratio is strong, and mobility is moderate, and plasticity-is good.
1.2, extrusion process
The plasticity wet feed the first step made or wet grain are put in extrusion machine, and the fashion of extrusion such as to roll by wet feed by the hole of tool certain diameter or sieve through screw propulsion or rolling, wherein hole sizer diameter selects 0.45mm, is squeezed into cylindrical strip extrudate.Extrude bar surface smooth, controlling extrudate temperature is 55 DEG C.
1.3, round as a ball one-tenth ball process
Be discharged on the rotation friction plate of spheronizator by above-mentioned extrudate heap, extrudate is then dispersed into the less right cylinder that length is equivalent to its diameter, and due to the effect of frictional force, these plastic cylindrical materials ceaselessly roll onboard, are rolled into spheroidal gradually.
2, enzyme ball dry coationg
The wet enzyme ball of preparation is placed in fluidized-bed, inlet temperature 45 DEG C-75 DEG C is set, air quantity 100m
3/ h-160m
3/ h, be dried to when temperature of charge reaches 45 DEG C-50 DEG C and carry out dressing, wherein the compound method of coating liquid is: be dissolved in after coating components sieves in water, is mixed with 4%-10% suspension and sieves, then fluidized-bed inlet temperature 45 DEG C-75 DEG C, air quantity 60m
3/ h-170m
3/ h, atomizing pressure 1.25bar-2.5bar.Coating type enzyme granulate is obtained after enzyme ball is coated.
After testing, in preparation process, enzyme activity loss is about 6.1%.
Embodiment 2
(1) material prepares
Material is prepared according to following listed parts by weight.
In enzyme ball, the parts by weight of each component are:
Enzyme component: alkaline lipase 55 weight part;
Stabilizer component: glucose 4.5 weight part, carboxymethyl cellulose 4.0 weight part, polyoxyethylene glycol PEG-15004.5 weight part, SODIUM PHOSPHATE, MONOBASIC 8 weight part, magnesium chloride 20 weight part, W-Gum 25 weight part.
In dressing, the parts by weight of each component are:
SODIUM PHOSPHATE, MONOBASIC 15 weight part, polyvinyl alcohol PEG-1000 8 weight part, PVP K30 20 weight part, magnesium chloride 12 weight part, starch 14 weight part, titanium dioxide 5 weight part, bright blue 0.05 weight part.
(2) coating type enzyme granulate is prepared
1, the making step of enzyme ball is as follows:
1.1, the preparation of wet feed
Enzyme and stablizer are shattered respectively, sieve after weigh in proportion, mix, add the aqueous solution as condensing agent or tackiness agent, the mass ratio of material and water is 4.5:1, after mixing wet feed.Use above-mentioned enzyme ball formula, wet feed moisture-retaining capacity obtained under this material-water ratio is strong, and mobility is moderate, and plasticity-is good.
1.2, extrusion process
The plasticity wet feed the first step made or wet grain are put in extrusion machine, and the fashion of extrusion such as to roll by wet feed by the hole of tool certain diameter or sieve through screw propulsion or rolling, wherein hole sizer diameter selects 0.45mm, is squeezed into cylindrical strip extrudate.Extrude bar surface smooth, controlling extrudate temperature is 65 DEG C.
1.3, round as a ball one-tenth ball process
Be discharged on the rotation friction plate of spheronizator by above-mentioned extrudate heap, extrudate is then dispersed into the less right cylinder that length is equivalent to its diameter, and due to the effect of frictional force, these plastic cylindrical materials ceaselessly roll onboard, are rolled into spheroidal gradually.
2, enzyme ball dry coationg
The wet enzyme ball of preparation is placed in fluidized-bed, inlet temperature 45 DEG C-75 DEG C is set, air quantity 100m
3/ h-160m
3/ h, be dried to when temperature of charge reaches 45 DEG C-50 DEG C and carry out dressing, wherein the compound method of coating liquid is: be dissolved in after coating components sieves in water, is mixed with 4%-10% suspension and sieves, then fluidized-bed inlet temperature 45 DEG C-75 DEG C, air quantity 60m
3/ h-170m
3/ h, atomizing pressure 1.25bar-2.5bar.Coating type enzyme granulate is obtained after enzyme ball is coated.
After testing, in preparation process, enzyme activity loss is about 8.4%.
Embodiment 3
(1) material prepares
Material is prepared according to following listed parts by weight.
In enzyme ball, the parts by weight of each component are:
Enzyme component: amylase 35 weight part;
Stabilizer component: glucose 2.5 weight part, carboxymethyl cellulose 3.0 weight part, polyoxyethylene glycol PEG-1500 6.5 weight part, SODIUM PHOSPHATE, MONOBASIC 14 weight part, magnesium chloride 15 weight part, W-Gum 20 weight part.
In dressing, the parts by weight of each component are:
SODIUM PHOSPHATE, MONOBASIC 10 weight part, polyvinyl alcohol PEG-1000 5 weight part, PVP K30 15 weight part, magnesium chloride 15 weight part, starch 25 weight part, titanium dioxide 6 weight part, bright blue 0.1 weight part.
(2) coating type enzyme granulate is prepared
1, the making step of enzyme ball is as follows:
1.1, the preparation of wet feed
Enzyme and stablizer are shattered respectively, sieve after weigh in proportion, mix, add the aqueous solution as condensing agent or tackiness agent, the mass ratio of material and water is 5:1, after mixing wet feed.Use above-mentioned enzyme ball formula, wet feed moisture-retaining capacity obtained under this material-water ratio is strong, and mobility is moderate, and plasticity-is good.
1.2, extrusion process
The plasticity wet feed the first step made or wet grain are put in extrusion machine, and the fashion of extrusion such as to roll by wet feed by the hole of tool certain diameter or sieve through screw propulsion or rolling, wherein hole sizer diameter selects 0.45mm, is squeezed into cylindrical strip extrudate.Extrude bar surface smooth, controlling extrudate temperature is 60 DEG C.
1.3, round as a ball one-tenth ball process
Be discharged on the rotation friction plate of spheronizator by above-mentioned extrudate heap, extrudate is then dispersed into the less right cylinder that length is equivalent to its diameter, and due to the effect of frictional force, these plastic cylindrical materials ceaselessly roll onboard, are rolled into spheroidal gradually.
2, enzyme ball dry coationg
The wet enzyme ball of preparation is placed in fluidized-bed, inlet temperature 45 DEG C-75 DEG C is set, air quantity 100m
3/ h-160m
3/ h, be dried to when temperature of charge reaches 45 DEG C-50 DEG C and carry out dressing, wherein the compound method of coating liquid is: be dissolved in after coating components sieves in water, is mixed with 4%-10% suspension and sieves, then fluidized-bed inlet temperature 45 DEG C-75 DEG C, air quantity 60m
3/ h-170m
3/ h, atomizing pressure 1.25bar-2.5bar.Coating type enzyme granulate is obtained after enzyme ball is coated.
After testing, in preparation process, enzyme activity loss is about 10.1%.
Embodiment 4
Enzyme component is replaced with: Sumizyme MP 10 weight part, cellulase 10 weight part, amylase 10 weight part and mannase 10 weight part; Other component is identical with embodiment 1 with technique.
After having prepared, detect the loss of preparation process neutral and alkali proteinase activity and be about 3.4%, amylase activity loss is about 5.3%.
Embodiment 5
Enzyme component is replaced with: alkaline lipase 10 weight part, cellulase 10 weight part, amylase 10 weight part and mannase 10 weight part; Other component is identical with embodiment 2 with technique.
After having prepared, detect the loss of preparation process neutral and alkali lipase activity and be about 4.5%, amylase activity loss is about 4.6%.
Comparative example 1
Material is prepared according to following listed parts by weight.
In enzyme ball, the parts by weight of each component are:
Enzyme component: Sumizyme MP 45 weight part;
Stabilizer component: dextrin 15 weight part, bean powder 25 weight part, lactose 1 weight part, sodium laurylsulfonate 3 weight part, carboxymethyl cellulose 6 weight part, W-Gum 20 weight part.
In dressing, the parts by weight of each component are:
Dextrin 30 weight part, starch 10 weight part, polyvinyl alcohol 15 weight part, sodium laurylsulfonate 1 weight part, sodium sulfate 20 weight part, titanium dioxide 20 weight part, bright blue 0.01 weight part.
Preparation technology and method, with embodiment 1, after having prepared, detect the loss of preparation process neutral and alkali proteinase activity and are about 18.6%.
Carry out quality examination to the product of preparation in embodiment 1-5 and comparative example 1, have detected homogeneity, solvability, weight loss on drying and stability respectively, detected result is as shown in table 1.
The quality examination of table 1 coating type enzyme granulate
Group |
Homogeneity |
Disintegration time |
Weight loss on drying |
Stability |
Embodiment 1 |
99% |
40s |
4% |
92% |
Embodiment 2 |
98% |
44s |
5% |
94% |
Embodiment 3 |
98% |
45s |
5% |
91% |
Embodiment 4 |
98% |
48s |
6% |
95%* |
Embodiment 5 |
98% |
40s |
6% |
96%** |
Comparative example 1 |
98% |
138s |
6% |
82% |
Note: * is in proteolytic enzyme; * is in lipase.
Adopt prescription of the present invention and coordinate wet-method extrusion prilling process of the present invention to prepare coating type enzyme granulate, achieve detersive enzyme safe, easy, prepare efficiently, achieve low dust or without dust granulation, improve the stability of production technique, reduce the impact of human factor on quality product and yield, in preparation process, enzyme activity is lost in about 4-8%, can maintain more than 90% 37 DEG C of enzyme work of preserving 9 months.Enzyme granulate and water are put into water with 1: 100 ratio, and room temperature lower magnetic force stirs low rate mixing, record enzyme granulate disintegration time.The disintegration time of this product granulated pellet, within 50s, is better than similar products at home and abroad, and random sampling 1kg, sieves with standard sieve, detects 30 order ~ 60 order particle accounting examples and arrives 98%.
The all documents mentioned in the present invention are quoted as a reference all in this application, are just quoted separately as a reference as each section of document.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read above-mentioned teachings of the present invention, these equivalent form of values fall within the application's appended claims limited range equally.