CN102443363A - Natural bonding agent adopting garlic and manufacture method thereof - Google Patents
Natural bonding agent adopting garlic and manufacture method thereof Download PDFInfo
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- CN102443363A CN102443363A CN2010105094990A CN201010509499A CN102443363A CN 102443363 A CN102443363 A CN 102443363A CN 2010105094990 A CN2010105094990 A CN 2010105094990A CN 201010509499 A CN201010509499 A CN 201010509499A CN 102443363 A CN102443363 A CN 102443363A
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Abstract
The invention relates to a method for manufacturing high-antibiosis natural bonding agents by using garlic as major ingredients, which comprises the following steps that: 1, the garlic is prepared, peeled and cleaned; 2, garlic pulp is obtained through the crushed and cleaned garlic; 3, water which is a polar solvent is added to the garlic pulp, and the weight of the water is twice or three times of the weight of the garlic; 4, liquid contents are extracted from a mixture of the garlic pulp and the water; 5, garlic extracts are obtained through the liquid contents extracted through filtering; and 6, the garlic extracts are concentrated to 50 to 70 Brix at the concentration temperature being 55 to 65 DEG C. In addition, the invention provides a natural bonding agent using the garlic, which is extracted, filtered and concentrated from a mixture of the crushed garlic and the water, wherein the light inspection drying time is 20 to 30 minutes at 20 DEG C, 14 to 24 minutes at 40 DEG C or 1 to 11 minutes at 60 DEG C, the pH is 6.0 to 7.0, the consistency viscosity is 100 to 2000 (cP), the nonvolatile matter content is 60 to 70 percent, the density is 1.0 to 1.3g/m<3>, and the peeling intensity at 180 DEG C is 12 to 16N/25mm.
Description
Background of invention
Description of Related Art
Generally speaking, tackiness agent is meant the material of the object that is used to combine identical or different kind fully, passes in time and adheres and from liquid curing and self ruined polymer substance seldom but typically refer to.
" bonding " of tackiness agent is different from " connection " because " bonding " with soaking, soak be since between tackiness agent and object each other similarity tackiness agent evenly infiltrate the effect of object along the interface between tackiness agent and object.More particularly; When tackiness agent " contact " object; It evenly infiltrates object along interface therebetween through " soaking "; Thereby tightly " combine " also " curing " with object according to machinery and chemical adhesion intensity (for example set effect, slide fastener effect, capillary effect and similar effect, they are the internal factors that produce bond strength).In case tackiness agent solidifies, it tightly keeps tacky state, and is irrelevant with the Externality such as temperature, humidity, pressure or similar factor.
Tackiness agent possibly be divided into inorganic adhesive and organic binder bond usually, and it can be subdivided into synthetic resin based, rubber-based and natural base.
On the other hand, recently, the infringement case increases suddenly, such as, such as, the sick room syndrome, headache, atopic dermatitis, asthma and the similar disease that cause by deleterious chemical such as formaldehyde or analogue.Sick room syndrome means the toxicity symptom that is caused like formaldehyde, acetaldehyde, toluene, YLENE, benzene, ethylbenzene, dichlorobenzene, vinylbenzene etc. by volatile organic compounds (" VOC "), and its major cause can find in the tackiness agent that contains such chemical, material of construction and analogue.
Therefore, recently, the demand of (if possible) so-called " natural glue " of the interpolation of eliminating volatile organic compounds and use is increased.
Yet,, be easy to by the inferior position of bacterium and analogue pollution just this natural glue has its anticorrosion variation if from natural glue, eliminate the use of volatile organic compounds fully.In view of this reason, existing tackiness agent contains a spot of anti-corrosion composition such as formaldehyde or analogue.In addition, volatile organic compounds is used to tackiness agent and restriction that resin, solvent, catalyzer, stiffening agent, additive and analogue as additive except that the tackiness agent staple are had no.
Therefore, volatile organic compounds volatilizees in drying that has tackiness agent now and process of setting, and produce carcinogens and also cause the disease infringement, for example sick room syndrome, for example, headache, atopic dermatitis, asthma and similar disease.
Invention field
The present invention relates to natural glue, and more particularly use the natural glue of garlic as the height-antibiosis of staple, with and method of manufacture.
Summary of the invention
The present invention is used for overcoming above problem, and the purpose of this invention is to provide and use natural materials such as the garlic nontoxic natural glue as the height-antibiosis of staple, and method of manufacture.
For reaching above purpose, according to an aspect of the present invention, a kind of method of using garlic to make natural glue is provided, comprising: first step, preparation, peeling and clean said garlic; Second step is obtained the garlic slurry through pulverizing the garlic that cleaned; Third step will add to said garlic slurry for the water of polar solvent, and said water is two times or three times of weight of said garlic; The 4th step, extracting liq composition from the mixture of said garlic slurry and said water; The 5th step is obtained the garlic extract through the liquid component that filters said extraction; And the 6th step, with 55～65 ℃ thickening temperatures with said garlic extract simmer down to 50～70 Brixs.
Preferably, said method also is included between third step and the 4th step polysaccharidase is added to the mixture of said garlic slurry and said water and in the Preset Time section, keeps first intermediate steps of this interpolation state.
Preferably, said polysaccharidase is a kind of in the fungal amylase of 0.04～0.12wt% of complex polysaccharide enzyme and garlic weight of 0.04～0.12wt% of garlic weight, and said Preset Time section is 30～120 minutes.
Preferably, said method also is included in second intermediate steps that adds one of at least browning inhibitor between the 4th step and the 5th step and after the 5th step.
Preferably, said browning inhibitor is a kind of in Hydrocerol A, sodium metabisulfite and the hexanodioic acid, and adds with 0.5～1.5wt% with respect to the weight of liquid component that extracts or garlic extract.
Preferably; Second step comprises the use homogenizer; The 5th step comprises that the liquid component through using separating centrifuge to filter extraction first obtains supernatant; And the strainer that uses 6-10 μ m then, the supernatant that the strainer secondary filtration of preferred 8 μ m is obtained, and the 6th step comprises the use rotary vacuum evaporator.
According to another aspect of the present invention; A kind of natural glue that uses garlic is provided, and said natural glue is extraction from the mixture of garlic of pulverizing and water, filtration and spissated, is 20 ℃ of 20～30 minutes, 40 ℃ following 1～11 minute of 14～24 minutes and 60 ℃ down down to X-ray examination X time of drying (candles drying time) wherein; PH is 6.0～7.0; Denseness viscosity is 100～2000 (cP), and non-volatile content is 60～70%, and density is 1.0～1.3g/m
3, and 180 ° of stripping strengths are 12～16N/25mm.
Because the garlic that uses good antibiosis has the advantage of high adhesive force and high antibiosis as staple according to the natural glue of use garlic of the present invention.
The accompanying drawing summary
In conjunction with accompanying drawing, above and/or other aspect of the present invention will become clear and be easier to understanding with advantage from the description of following embodiment, wherein:
Fig. 1 is the schema of the method for explanation natural glue constructed in accordance;
Fig. 2 shows the test picture of the natural glue of first embodiment according to the present invention to the antibiosis characteristic of bacterium;
Fig. 3 shows the test picture of the natural glue of second embodiment according to the present invention to the antibiosis characteristic of mould;
Fig. 4 to Fig. 6 is the figure that shows the variation of the polysaccharidase kind depend on the natural glue of the 3rd embodiment according to the present invention and the Hunter value of extraction time;
Fig. 7 to Figure 11 shows that the brown stain of depending on the browning inhibitor kind of the natural glue of the 4th embodiment according to the present invention suppresses the figure that renders a service;
Figure 12 to Figure 16 shows that the brown stain of depending on the browning inhibitor kind of the natural glue of the 4th embodiment according to the present invention suppresses the figure of speed;
Figure 17 and Figure 18 show that the brown stain of depending on the shelf time of the natural glue of the 4th embodiment according to the present invention suppresses the figure that renders a service; And
Figure 19 and Figure 20 show the brown stain retarding effect of the browning inhibitor (sodium metabisulfite) of the natural glue of the 4th embodiment and the figure of denseness viscosity according to the present invention.
Detailed description of the preferred embodiments
Fig. 1 is the schema that explanation garlic used according to the invention is made the method for natural glue (since then abbreviating " natural glue " as).With reference to figure 1, at first will be described below a preferred aspect using garlic to make the natural glue method.
At first step, prepare garlic (st1).The garlic of preparing is the common living garlic that is easy to from the market acquisition.After the peeling, with washing garlic with get on from the garlic removal of impurity such as earth, root, branch, leaf and analogue.
In second step, pulverize the garlic that cleaned and starch (st2) to obtain garlic.Be purpose easily, can use homogenizer to pulverize garlic as far as possible subtly so that its granularity can be little.Obtained the garlic slurry thus.
At third step, solvent is added in the garlic of pulverizing (st3).Institute's solubilizing agent can be the polar solvent such as water, and it is with every 1g garlic 2～3ml, and the ratio of preferred 2.5ml adds.The kind of solvent for use is considered productive rate with amount.
In the 4th step, extracting liq composition (st4) from the mixture of water and garlic slurry.Extract after solvent began to experience 1-3 hour preferred 2 hours from adding, and the temperature maintenance that makes mixture at the time durations of experience is at 20～30 ℃ preferred 25 ℃.Experience 2 hours was to consider absorbancy and the Hunter value of institute's extracting liq composition and specified before extracting, and the temperature of prescribed mixt is to minimize brown stain effect or caramelization.
In the 5th step, filter the liquid component (st5) that is extracted.Once filter with separating centrifuge and/or strainer, preferably carry out twice filtration.If necessary, the liquid component that uses separating centrifuge to filter said extraction first obtains supernatant, and uses the strainer of 6-10 μ m then, the strainer of preferred 8 μ m, the supernatant that secondary filtration obtained.Therefore obtain garlic extract and residue.
In the 6th step, with 55～65 ℃, preferred 60 ℃ thickening temperature is 50～70 Brixs with garlic extract vacuum concentration (st6), preferred 60 Brixs.Rotary vacuum evaporator can be used for concentrating.
Thus, accomplished natural glue of the present invention.
Consider natural glue material different performance of the present invention; To X-ray examination X is 20 ℃ of 20～30 minutes, 40 ℃ 14～24 minutes and 60 ℃ 1～11 minute down down down time of drying; PH is 6.0～7.0; Denseness viscosity is 100～2000 (cP), and non-volatile content is 60～70%, and density is 1.0～1.3g/m
3, and 180 ° of stripping strengths are 12～16N/25mm.The definition of these material properties and implication will be explained in more detail at relevant portion.
Simultaneously, in above-mentioned technology, preferably, insert first intermediate steps (st11) that polysaccharidase is added to the mixture of garlic slurry and water between solvent interpolation in third step and the extraction in the 4th step.The instance of polysaccharidase can comprise the fungal amylase of 0.04～0.12wt% of complex polysaccharide enzyme, the garlic weight of 0.04～0.12wt% of garlic weight.Preferably, the plain enzyme of complex polysaccharide that adds the 0.04wt% of garlic weight.Add and extract between time period be, for example, 30～120 minutes, preferred 120 minutes.The reason of adding polysaccharidase is to consider productive rate.
In addition, preferably, second intermediate steps (st21) that browning inhibitor is added to liquid and/or the spissated liquid of extraction is inserted between the concentrating in extraction and the 5th step in the 4th step and/or is added in after the concentrating in the 5th step.The instance of browning inhibitor can comprise Hydrocerol A, sodium metabisulfite and the hexanodioic acid of 0.5～1.5wt% of institute's extracting liq and/or institute's concentrating liquid weight.Preferably, the sodium metabisulfite that adds the 1.0wt% of institute's extracting liq or institute's concentrating liquid weight.The reason that adds browning inhibitor is to consider the distinctive brown stain effect of garlic.
First to the 8th experimental embodiment that will describe the natural glue of first embodiment hereinafter and be used for its material property according to the present invention.
First embodiment
Korea S's South Sea garlic is cleaned and pulverizes to obtain 1kg garlic slurry with homogenizer.After adding the 2.5L tri-distilled water, with the garlic slurry that is obtained in shaking bath, remain on 25 ℃ 2 hours, and afterwards from the garlic slurry with the VELOCITY EXTRACTION liquid component of 380rpm.Afterwards; (7,000rpm/30min) filtration obtains supernatant first, and (Whatman numbers 2 through 8 μ m strainers with this supernatant afterwards through separating centrifuge with this liquid component; 8) secondary filtration; And at last the filtering supernatant of institute is maintained at 60 ℃ and vacuum concentration is 60 ° of Brixs in rotary vacuum evaporator (deriving from Eyela, Rikakikai Co., Japan).
To in following first to the 8th experimental embodiment, one after the other describe to X-ray examination X time of drying, pH, denseness viscosity, non-volatile content, density, 180 ° of stripping strengths, to the antibiosis characteristic of bacterium with to the antibiosis characteristic of mould, all these performances are main raw performances of the natural glue of this embodiment.
< the first experimental embodiment >: to X-ray examination X time of drying
Term " to X-ray examination X time of drying " is used to find out the liquid dried time, its mean up to when contact liq coating surperficial the time, can not detect in one's hands in time of liquid.
In this experimental embodiment, select and the neat colourless and transparent plate glass in cutting both sides.Then, the section of cutting glass is polished through grinding stone such as emery dust,, in alkali lye boiling water, cleans then such as soap, washing composition or analogue so that it becomes circle, and at last with the mixture cleaning of ethanol and toluene down to dustless.As use new plate glass, then with its be dipped in 90% or more highly purified SRM 935a and sulfuric acid mixture liquid in 24 hours or more for a long time and after clean.Then; Will be according to the present invention the 3g natural glue of first embodiment drop on the plate glass; And be coated with uniform thickness with knifing machine above that afterwards with uniform force degree and speed (150mm/sec); And measure and when keeping steady temperature (20 ℃, 40 ℃ and 60 ℃) and constant humidity, use finger can not feel the time of adhering under the constant timed interval.
< the second experimental embodiment >: pH
In this experimental embodiment, will be according to the present invention the natural glue of first embodiment with the equivalent distilled water diluting after, its pH measures several times with pH meter under 25 ± 1 ℃, and the mean number of institute's measured value shows with a decimal place.
< the 3rd experimental embodiment >: denseness viscosity
The denseness viscosity of tackiness agent is the factor directly related with workability, and interrelated with non-volatile content and molecular-weight average, and its variation is the criterion of storage stability.
In this experimental embodiment; The denseness viscosity of the natural glue of first embodiment is keeping under 20 ℃ the envrionment temperature with viscometer (Brookfield model DV-I+ according to the present invention; The rotation number of 100rpm (rotating shaft numbering 2)) measure twice, and its MV is represented with centipoise (cP=P/100).
< the 4th experimental embodiment >: non-volatile content
Non-volatile content representes that this is the material that produces actual adhesion power through the weight of residuals behind the heated adhesive removal volatile matter.
In this experimental embodiment, prepare the foil disk of diameter 4.5cm and accurately claim its weight (W0 (g)), and, place this dish upward the natural glue of 1.5g first embodiment according to the present invention after, measure its weight (W1 (g)).Then, after 180 ± 5 minutes, sample cools off in containing the moisture eliminator of siccative also measures its weight (W3 (g)) then at 105 ± 1 ℃ of down dry these natural glues of hot air circulation type steady temperature.This program is repeated secondary or more times, and represent with two position effective digitals according to the result's of following equation 1 MV.
Equation 1: non-volatile content (%)={ (W2-W0)/(W1-W0) } * 100
< the 5th experimental embodiment >: density
In this experimental embodiment; In holding temperature is under 20 ± 0.5 ℃; Will be according to the present invention the natural glue of first embodiment put into known weight big graduated cylinder (mass cylinder) (100m1); No bubble adds to 100ml, and (counterweight 500g, loss of weight 0.5g) measures its weight to use balance afterwards.The density of natural glue is pressed following equation 2 and is calculated.
Equation 2:S=(W1-W2)/100
Wherein, S: density (g/m
3), W1: the gross weight (g) of reference sample and big graduated cylinder, and W2: the weight (g) of big graduated cylinder.
< the 6th experimental embodiment >: 180 ° of stripping strengths
In this experimental embodiment, prepare the thick clamping plate of the 5mm-of leakless or crackle (125 * 150mm), with brush will be according to the present invention the natural glue of first embodiment with 50g/m
2For unit evenly coats on these clamping plate.After 5 minutes, with the cotton (117g/m of 175 * 150mm
2) be covered on the natural glue of coating, and, with cylinder the cotton that covers is being applied under the heavy burden of 49N, cotton is unidirectional but not press five times two-wayly, then sample was placed 48 hours according to present appearance, simultaneously sample is remained in 20 ℃ the environment.After this; Is that at interval make cut channel form 5 test specimens on the clamping plate surface with 25mm through using bite or analogue; Each test specimen cotton on one side is stripped to 50mm; The cotton of clamping plate and corresponding section is connected in the anchor clamps of tension tester, and the interval between anchor clamps becomes about 10mm with the length that the speed of 200mm/min increases until the tackiness agent part of test specimen, and mensuration is according to the value of the tension load value of peeling off of test specimen; And afterwards the MV of the maximum tension load value of broken parts is used as 180 ° of stripping strengths, shows with N/25mm.
Following table 1 shows the result of above first to the 6th experimental embodiment.
[table 1]
As a reference; In existing tackiness agent; Starch-based has the average 180 ° of stripping strengths of 8.4 (N/25mm) and average 16.5% non-volatile content, and PVAc (polyvinyl acetate) has the average 180 ° of stripping strengths of 17.5 (N/25mm) and average 30% non-volatile content, and Pleuran is a microorganism agent; It has 8.0% average non-volatile content, and the microcapsule essential oil has 30.0% average non-volatile content.Thus, the bond strength of the natural glue of first embodiment is higher than the bond strength of starch-based and is lower than the bond strength of PVAc slightly according to the present invention, but non-volatile content is significantly different with starch-based and PVAc.In a word, can not increase non-volatile content again, can find out that natural glue performance according to the first embodiment of the present invention is better relatively owing to having the reduction of tackiness agent now because of workability.
< the 7th experimental embodiment >: to the antibiosis characteristic of bacterium
In this experimental embodiment, be on the basis of agar diffusion method, to measure to the antibiosis activity of bacterium.That is to say; Harmful microbe water culture medium shown in the following table 2 is inoculated in the Muller Hinton substratum that contains 0.6% soft agar with 50 μ l respectively and mixes well, and on the Mueller Hinton plating medium for preparing in advance, processes bilayer afterwards.After this, with 1,3,5,7 and the natural glue of first embodiment of 9mg/ml according to the present invention suck paper disc (derive from Toyo Rhosikaisha, Ltd be 8mm) to place double-deck substratum to cultivate at the constant temperature appearance that is set at 35 ℃.In this case, measure the zone clearly that shows that the blocking-up harmful microorganism is cultivated.
[table 2]
Measure the result and see Fig. 2.The bacterium that is used to detect is following, and each lowercase in Fig. 2, a to e, the amount of representative natural glue of first embodiment according to the present invention, it is (a) 1mg/ml successively, (b) 3mg/ml, (c) 5mg/ml, (d) 7mg/ml and (e) 9mg/ml.
A, Bacillus cereus (Bacillus cereus) KCCM-11204
B, intestinal bacteria (Escherichia coli) ATCC-25922
C, Pseudomonas aeruginosa (Pseudomonas aeruginosa) ATCC-15442
D, streptococcus aureus (Staphylococcus aureus) KCTC-1927
E, Salmonella typhimurium (Salmonella typhiumurium) KCTC-2208
F, Vibrio parahemolyticus (Vibrio parahaemolyticus)
It is active that the natural glue of having confirmed first embodiment according to the present invention shows high antibiosis generally; Especially; It is active that intestinal bacteria, Pseudomonas aeruginosa and Salmonella typhimurium are shown high antibiosis; It begins these bacterium are shown antibiosis and keeping high antibiosis up to 3～9mg/ml from 1mg/ml, and begins Bacillus cereus, streptococcus aureus and Vibrio parahemolyticus are shown antibiosis from 3mg/ml.
< the 8th experimental embodiment >: the antibiosis to fungi is active
In this experimental embodiment; Sterile distilled water is allocated in the fungal bacterial strain of on plating medium, cultivating shown in the following table 3 with suspension fungi (Foggia) with 9ml, and 1ml fungi liquid (Foggia liquid) is made into bilayer in the double-deck substratum of the PDA that contains 0.6% soft agar afterwards.After this, with 1,3,5 and the natural glue of first embodiment of 7mg/ml according to the present invention suck paper disc respectively (derive from Toyo Rhosikaisha, Ltd be 8mm) to place double-deck substratum to cultivate at the constant temperature appearance that is set at 35 ℃.In this case, measure the zone clearly that shows that the blocking-up harmful microorganism is cultivated.
[table 3]
Measure the result and see Fig. 3.The fungi that is used to detect is following, and each lowercase in Fig. 3, and a to d represents the amount of natural glue, and it is (a) 1mg/ml successively, (b) 3mg/ml, (c) 5mg/ml and (d) 7mg/ml.
A, mucor javanicus (Mucor javanicus) AM-2
B, penicillium spp (Penicillium sp.)
C, black mold (Aspergillus niger) IFO-31125
D, Rhizopus microsporus (Rhizopus microsporus) KCTC-6969
The natural glue of having confirmed first embodiment according to the present invention shows the high antibiosis of fungi active generally, and especially, it is active when 5mg/ml concentration, to show high relatively antibiosis.Especially, it is active when 7mg/ml concentration, penicillium spp to be shown the highest antibiosis.
The natural glue of several different embodiments will one after the other be described below according to the present invention.
Second embodiment
This embodiment is interrelated with third and fourth step of method of manufacture shown in Figure 1, and introduces the several experimental embodiment about solvent species and amount, extraction time and extraction temperature.It should be noted that in this embodiment unspecified content is identical with content in first embodiment.
< the first experimental embodiment >: depend on and extract solvent species and productive rate and the absorbancy of extracting temperature
The water of 2.5 times of garlic weight and 8 kinds of organic solvents are added in the garlic slurry, and respectively under 25 ℃, 30 ℃, 40 ℃ and 50 ℃ from wherein extracting garlic one hour with relatively solid productive rate and absorbancy.Result relatively is as shown in table 4.
[table 4]
From table, can find out that the solid productive rate descends with following order: peaked water 45.0～47.1%, methyl alcohol 25.3～37.2%, ethanol 20.1～28.3%, Virahol 12.6～14.7% and acetone 7.0～11.8%.In contrast, diethyl ether, normal hexane, vinylchlorid and the methylene dichloride for non-polar solvent has low-down solid productive rate.
The solid productive rate tends to increase with temperature.Along with temperature rises to 50 ℃ from 25 ℃, the solid productive rate for water increase about 2% (from 45.0% to 47.1%), for methyl alcohol increase about 12%, for ethanol increase about 10%, increase about 2.0% and increase about 4% for Virahol for acetone.In contrast, non-polar solvent does not have on the solid productive rate obviously increases.
For the absorbancy of measuring at 600nm, glassware for drinking water has 0.15～0.18 mxm..Methyl alcohol, ethanol, Virahol and acetone have 0.33～0.50,0.010～0.040,0.005～0.024 and 0.008～0.026 value respectively, show that polar solvent has more high absorbance than non-polar solvent.
Increase descends absorbancy at each temperature from 25 ℃ to 50 ℃ with water temperature.In contrast, the dewater absorbancy of outer remaining solvent increases with temperature.
< the second experimental embodiment >: depend on and extract solvent types and productive rate, absorbancy and the Hunter value of extracting temperature
Water, methyl alcohol, ethanol, Virahol and acetone (they are to have the solvent of high solid productive rate and are 2.5 times of garlic weight) are added to the garlic slurry, and with being set at 25 ℃ extraction temperature and observing productive rate, absorbancy and Hunter value with the extraction time that changed in 2,4 and 6 hours.Observed result is as shown in table 5.
[table 5]
Increase solid productive rate with extraction time reduces slightly.Water increases slightly after 4 hours and reduces slightly after 6 hours in experience in experience, but the remaining solvent no significant difference.
For the Hunter value, " L " is worth every kind of solvent no significant difference, and " a " value increases smallly and produce darker green.
< the 3rd experimental embodiment >: the productive rate, denseness viscosity, Hunter value and the bond strength that depend on the water yield
The effect that depends on productive rate, denseness viscosity, Hunter value and the bond strength of the water yield for research; 2.5 times, 3 times, 4 times of garlic weight and 5 times water are added to the garlic slurry; Then 25 ℃ extraction temperature; 2 hours extraction time, extract number and be under 1 and 60 ℃ the condition of thickening temperature, comparison productive rate, denseness viscosity, Hunter value and bond strength 30 days.Comparative result is as shown in table 6.
[table 6]
Along with the water that is added into garlic slurry for the ratio of garlic weight with 1: 2.5,1: 3,1: 4 during with increase in 1: 5; The amount of tackiness agent is reduced to 320mL from 355mL; The denseness viscosity of the natural glue of accomplishing increases to 1 from 654.5cP; 309cP is total and the variation of Hunter value reduces with the increase of solvent ratios smallly.
Along with the adding proportion of water to garlic increased with 1: 2.5,1: 3 and 1: 4,180 ° of stripping strengths are shown as 15～17N/25mm, but when 1: 5 adding proportion, slightly drop to 13～16N/25m.
< the 4th experimental embodiment >: the amount that depends on extraction time and the garlic residue that extracts temperature
The water of 2.5 times of garlic weight is added in the garlic slurry, to the extraction conditions of extraction time of the extraction temperature of 25 ℃, 30 ℃, 40 ℃ and 50 ℃ and 0,1,2,4 and 6 hour down behind the liquid mixture secondary filtration of extraction the amount of remaining garlic residue compare.Comparative result as shown in Figure 3.
Can find out that from this figure even when extracting temperature with the extraction time increase, the amount of garlic residue does not have remarkable change yet.Yet browning degree increases along with extracting temperature and the increase of extraction time.
Summarize above-mentioned first to the 4th experimental embodiment; The solvent that when natural glue constructed in accordance, adds to the garlic slurry is preferably, to be the water of polar solvent; Water is preferably 1: 2.5 for the adding proportion of garlic weight; Extract temperature and be preferably 25 ℃, and extraction time is preferably 2 hours, as shown in table 7 below.
[table 7]
| The extraction temperature (℃) | Extraction time (hr) | Extract solvent | Garlic-solvent ratio of pulverizing | Water cut | Garlic extract productive rate |
| 25 | 2 | Water | 1kg-2.5 |
60～63％ | 45.0％ |
The 3rd embodiment
This embodiment is interrelated with first intermediate steps (st11) in Fig. 1 method of manufacture, and introduces the several experimental embodiment about polysaccharidase kind, addition and interpolation time.It should be noted that in this embodiment unspecified content is identical with content in first embodiment.
< the first experimental embodiment >: depend on the variation of the Hunter value of polysaccharidase kind and extraction time
In this experimental embodiment, with 0.04wt%, 0.08wt% and 0.12wt% (garlic weight) for the complex polysaccharide enzyme of polysaccharidase and fungal amylase add to respectively in the mixture of garlic slurry and water, and 30～120 minutes Hunter value of comparison.Shown in comparative result such as Fig. 4 to 6.
As shown in Figure 4, along with the concentration of polysaccharidase and the increase in reaction times, the dL value is by-62.7 to-62.0 just (+) increases, and it shows as whiteness increases.As shown in Figure 5, along with the increase by 30 to 120 minutes of polysaccharidase concentration and reaction times, the da value is increased by-3.0 to-4.2 negative (-), shows as green variable color.As shown in Figure 6, the db value is 7.6 to 8.5, show with the experience time do not have considerable change.In other words, white is faded and green is faded along with the increase in polysaccharidase reaction times occurs.
< the second experimental embodiment >: the productive rate that depends on polysaccharidase kind and extraction time
In this experimental embodiment; With adding to respectively in the mixture of garlic slurry and water for the complex polysaccharide enzyme of polysaccharidase and fungal amylase of 0.04wt%, 0.08wt% and 0.12wt% (garlic weight); Keep sample and extract garlic after 30 to 120 minutes, and compare solid productive rate and Hunter value then.Comparative result is as shown in table 8.
[table 8]
Can find out that by last table for the complex polysaccharide enzyme, though along with the reaction times increased to 120 minutes by 30 minutes, the solid productive rate increases to 21.5% by about 7.18%, and along with the increase solid productive rate of complex polysaccharide enzyme concn does not have obvious increase.For fungal amylase, with the increase of amylomycin enzyme concn, the solid productive rate increases to 20.0% by about 3.0%.
< the 3rd experimental embodiment >: the component concentration that depends on the polysaccharidase kind changes
In this experimental embodiment, depend on that for research three control groups are compared in the component concentration variation of polysaccharidase kind.Experience after 2 hours in room temperature from garlic extraction first control group the mixture of slurry and the zero(ppm) water of 5 times of garlic weight; Temperature in 100 ℃ after experiencing 2 hours is extracted second control group from the mixture of the zero(ppm) water of garlic slurry and 5 times of garlic weight; And experience after 2 hours in the temperature of 45 ℃ (they be the optimal reaction temperature of enzyme) from garlic extraction the 3rd control group the mixture of the complex polysaccharide enzyme of the 0.04wt% of the zero(ppm) water of slurry, 5 times of garlic weight and garlic weight.Comparative result is as shown in table 9.
[table 9]
First and second control groups contain the glucose of 0.000wt% and 0.009wt% respectively; The fructose that contains 0.332wt% and 0.298wt% respectively; Contain the sucrose of 0.025wt% and 0.135wt% respectively and contain the SANMALT-S of 0.000wt% and 0.033wt% respectively, show and depend on the fructose content no significant difference that extracts temperature.The 3rd control group contains the glucose of 0.065wt%, the fructose of 0.913wt%, and the sucrose of 0.044wt% and the SANMALT-S of 0.034wt% show that fructose content is than the fructose content high 50% of first and second control groups or more.
Summarize above first to the 3rd experimental embodiment, in first intermediate steps of natural glue constructed in accordance, add with respect to the complex polysaccharide enzyme of the 0.04wt% of garlic weight and set by the time period that is added into extraction be 120 minutes be preferred.
The 4th embodiment
This embodiment is interrelated with second intermediate steps (st21) of the method for manufacture of Fig. 1, and introduces the several experimental embodiment about kind, addition and the interpolation time of browning inhibitor.It should be noted that in this embodiment unspecified content is identical with content in first embodiment.
< the first experimental embodiment >: the kind of browning inhibitor
In this experimental embodiment, respectively xitix, Hydrocerol A, L-halfcystine, sodium metabisulfite and the hexanodioic acid of 1～5w% added to the mixture of garlic slurry and water, and detect the browning degree of 0～60 day sample.Detected result is as shown in table 10.
[table 10]
Suppress although xitix has the most effectively brown stain at initial period, pass the brown stain effect in time and become serious.The material that demonstrated the highest brown stain inhibition at 60 days is Hydrocerol A, sodium metabisulfite, hexanodioic acid.
< the second experimental embodiment >: the brown stain of depending on the browning inhibitor kind suppresses to render a service
In this experimental embodiment, xitix, Hydrocerol A, L-halfcystine, sodium metabisulfite and the hexanodioic acid with 1～5wt% adds in the mixture of garlic slurry and water respectively, and detects the brown stain inhibition effectiveness of 0～60 day sample.Shown in detected result such as Fig. 7 to Figure 11.
As shown in Figure 7, to add for 1wt%, the brown stain inhibition effectiveness of xitix is passed in time and is reduced.Add for 2～5wt%,, pass brown stain in time and suppress to reduce to 8～15% suddenly from 60～70% though initial inhibition is renderd a service to about 60～65%.
As shown in Figure 8, add for 1～5wt%, the initial brown stain of Hydrocerol A suppresses to render a service up to 75～85%, and reduce to slightly after experiencing 30 days 41～57% and experience 60 days after reduce to 35～50%.
As shown in Figure 9, along with being increased by 1wt% to 5wt%, the brown stain of L-halfcystine suppresses effectiveness and reduces by half.
Shown in figure 10, to add for 1～5wt%, the initial brown stain of sodium metabisulfite suppresses to render a service up to 84～96%, reduce to 54～66% and 30～36% respectively when 30 days and 60 days, and the increase with addition reduces by half after 30 days.
Shown in figure 11, the initial brown stain of hexanodioic acid suppresses to render a service up to 64～73%, reduces to 7% to 43% scope after 60 days and experience.
< the 3rd experimental embodiment >: the brown stain of depending on the browning inhibitor kind suppresses speed
In this experimental embodiment, respectively xitix, Hydrocerol A, L-halfcystine, sodium metabisulfite and the hexanodioic acid of 1～5wt% added to the mixture of garlic slurry and water, and detect the brown stain inhibition speed of 0～60 day sample with 20 days interval.Brown stain suppress speed by first order reaction formula definition: ln (C/C0)=-Kt.Shown in detected result such as Figure 12 to 16.
Shown in figure 12, it is all very high up to 0～20 day that the brown stain of xitix suppresses speed, but fall suddenly after 20 days and after 40 days, have (-) value.
Shown in figure 13, it is all very high up to 0～20 day that the brown stain of Hydrocerol A suppresses speed, but descend up to 40 days and have (-) value, and increase slightly up to 40～60 talentes.
Shown in figure 14, it is the highest when 1wt% adds that the brown stain of L-halfcystine suppresses speed, but when 2～5wt% adds, during 40～60 days, generally reduce.
Shown in figure 15, it is constant in 0～60 day that the brown stain of sodium metabisulfite suppresses speed.
Shown in figure 16, it all was the highest up to 0～20 day that the brown stain of hexanodioic acid suppresses speed, but fell suddenly after 20 days.
< the 4th experimental embodiment >: depend on the variation of Hunter value of the kind of browning inhibitor
In this experimental embodiment; Following compound is added to the mixture of garlic slurry and water, and observe the Hunter value of 0～60 day sample: the 7th kind of compound and 3% (w/v) hexanodioic acid of the 5th kind of compound, 3% (w/v) sodium metabisulfite of the third compound, 3% (w/v) L-halfcystine of first kind of compound of 3% (w/v) xitix, 3% (w/v) Hydrocerol A and second kind of compound of 1% (w/w) xitix blended, 3% (w/v) L-halfcystine and 1% (w/w) xitix the 4th kind of compound, 3% of blended (w/v) sodium metabisulfite and 1% (w/v) xitix the 6th kind of compound, 3% of blended (w/v) hexanodioic acid and the 8th kind of compound of 1% (w/v) sodium metabisulfite blended.Detected result is as shown in table 11.
[table 11]
The Δ E that adds 3% (w/v) L-halfcystine separately is 12.41, and the Δ E of combination interpolation 3% (w/v) L-halfcystine and 1% (w/w) xitix is 1.88.
The Δ E that adds 3% (w/v) sodium metabisulfite separately is 1.10, and the Δ E of combination interpolation 3% (w/v) sodium metabisulfite and 1% (w/v) hexanodioic acid is 45.46.
The Δ E that adds 3% (w/v) hexanodioic acid separately is 3.76, and the Δ E of combination interpolation 3% (w/v) hexanodioic acid and 1% (w/v) sodium metabisulfite is 2.84.
Can find out by The above results; 3% (w/v) L-halfcystine is added in combination and 1% (w/w) xitix produces high synergistic effect; Independent Hydrocerol A, sodium metabisulfite and the hexanodioic acid of adding produces high effect, and adds sodium metabisulfite separately and make up the brown stain inhibition effectiveness of adding sodium metabisulfite and hexanodioic acid the highest.
< the 5th experimental embodiment >: the brown stain of depending on storage temperature suppresses to render a service
In this experimental embodiment; 100ml garlic extracting solution is mixed with 100ml zero(ppm) water; And mix with Hydrocerol A, L-halfcystine, sodium metabisulfite and the hexanodioic acid of 3% (w/v) respectively afterwards, and suppress to render a service 60 days in the brown stain of 4 ℃, 30 ℃ and 37 ℃ test sample.Shown in detected result such as Figure 17 and 18.
Generally speaking, brown stain suppresses to render a service to be increased with temperature, and sodium metabisulfite has than the better brown stain inhibition of Hydrocerol A, L-halfcystine and hexanodioic acid effectiveness.
< the 6th experimental embodiment >: depend on the variation of the Hunter value of period of storage
In this experimental embodiment, respectively 0～5% xitix, Hydrocerol A, L-halfcystine, sodium metabisulfite and hexanodioic acid added to the mixture of garlic slurry and water, and detect the variation of the Hunter value of 0～60 day sample.Detected result is as shown in Table 12.
[table 12]
Up to 0～10 day, total xitix has about 1.98～4.06 little Hunter value, it increased significantly with concentration and changes.
Up to 0～60 day, Hydrocerol A had total Hunter value of about 4.29～12.0, and it keeps stable in 0～60 day period of storage, and the total Hunter value when adding 1% Hydrocerol A is 1.18～5.46.
Up to 0～60 day, the L-halfcystine had total Hunter value of 6.39～11.1, and total Hunter value significantly becomes 13.2～17.5 when adding the 1wt%L-halfcystine.
Up to 0～60 day, sodium metabisulfite had total Hunter value of 5.42～12.2, and the total Hunter value when adding the 1w% sodium metabisulfite is 1.10～2.75, and inhibition is stablized in the variation of Hunter value when adding 2～5wt% sodium metabisulfite.
Up to 0～60 day, hexanodioic acid had total Hunter value of 5.43～12.3, and the total Hunter value when adding the 1w% hexanodioic acid is 1.75～2.30, obtained similar results when adding 2～3wt% hexanodioic acid.
< the 7th experimental embodiment >: the interpolation time of depending on the browning inhibitor kind
In this experimental embodiment; When respectively 0.5%, 1% and 2% sodium metabisulfite being added to the garlic extracting solution and again with it when concentrated; Detect brown stain and suppress (spectrophotometer, the U.S., 420nm) variation of effectiveness and denseness viscosity (Brookfield DV-III).
Although do not show among the figure; When placing the natural glue according to the present invention that does not add sodium metabisulfite on a piece of paper, can observe distortion, crack and brown tectum; But after the sodium metabisulfite with 0.5wt%, 1.0wt% and 1.5wt% added to this natural glue, applicability and similar performance were improved and do not have distortion and crack appearance.
Shown in figure 19, the brown stain of sodium metabisulfite suppresses to render a service for about 50%, when adding 0.5wt%, is 0.049, be 0.0286 to be 0.0316 when adding 2.0wt% when adding 1.0wt%, and shown in figure 20, denseness viscosity does not have considerable change.
In addition; In this experimental embodiment; Before concentrating and after concentrating; Promptly between the concentrating in extraction in the 4th step of Fig. 1 and the 5th step with the 5th step in concentrate after, hexanodioic acid and sodium metabisulfite are added to according to natural glue of the present invention, and Hunter value and the brown stain of detection in period of storage.Detected result is as shown in table 13.
[table 13]
For hexanodioic acid, variation, brown stain and the green of total Hunter value faded and before concentrating, added than adding more serious in concentrated back.
For sodium metabisulfite, the variation of total Hunter value is added before concentrating with brown stain and is added similar in concentrated back.
Summarize above first to the 7th experimental embodiment, the sodium metabisulfite that in natural glue of the present invention, adds one of at least with respect to the 1.0wt% of extracting solution and/or liquid concentrator weight after the concentrating between the concentrating in extraction in the 4th step of Fig. 1 and the 5th step and in the 5th step is preferred.
Though with reference to exemplary special exhibition of the present invention with the present invention has been described, one skilled in the art should appreciate that and can make the multiple change on form and the details and not deviate from the spirit and scope of the present invention it.It is for the present invention rather than restrictive meaning are described that exemplary is provided.Therefore, this invention is intended to comprise improvement of the present invention and variation, condition is that they are in the scope of appending claims and equivalent thereof.
Claims (7)
1. method of using garlic to make natural glue comprises:
First step: preparation, peeling and clean said garlic;
Second step: obtain the garlic slurry through pulverizing the garlic that cleaned;
Third step: will add to said garlic slurry for the water of polar solvent, said water is two times or three times of weight of said garlic;
The 4th step: extracting liq composition from the mixture of said garlic slurry and said water;
The 5th step: obtain the garlic extract through filtering the liquid component that is extracted; And
The 6th step: with 55～65 ℃ thickening temperatures with said garlic extract simmer down to 50～70 Brixs.
2. method according to claim 1 also is included between said third step and said the 4th step polysaccharidase is added to the mixture of said garlic slurry and said water and in the Preset Time section, keeps first intermediate steps of this interpolation state.
3. method according to claim 2, wherein said polysaccharidase are a kind of in the fungal amylase of 0.04～0.12wt% of complex polysaccharide enzyme and garlic weight of 0.04～0.12wt% of garlic weight, and said Preset Time section is 30～120 minutes.
4. method according to claim 1 also is included in second intermediate steps that adds one of at least browning inhibitor between said the 4th step and said the 5th step and after said the 5th step.
5. method according to claim 1, wherein said browning inhibitor are a kind of in Hydrocerol A, sodium metabisulfite and the hexanodioic acid, and add with 0.5～1.5wt% with respect to the weight of the liquid component of said extraction or said garlic extract.
6. method according to claim 1; Wherein said second step comprises the use homogenizer; Said the 5th step comprises that the liquid component through using separating centrifuge to filter said extraction first obtains supernatant, and uses the strainer of 6-10 μ m then, the strainer of preferred 8 μ m; The supernatant that secondary filtration obtained, and said the 6th step comprises the use rotary vacuum evaporator.
7. natural glue that uses garlic; Said natural glue is extraction from the mixture of garlic of pulverizing and water, filtration and spissated; Be time of drying 20 ℃ of 20～30 minutes, 40 ℃ 14～24 minutes and 60 ℃ 1～11 minute down down down to X-ray examination X wherein, pH is 6.0～7.0, and denseness viscosity is 100～2000 (cP); Non-volatile content is 60～70%, and density is 1.0～1.3g/m
3, and 180 ° of stripping strengths are 12～16N/25mm.
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| CN 201010509499 CN102443363B (en) | 2010-10-14 | 2010-10-14 | Natural bonding agent adopting garlic and manufacture method thereof |
| HK12109658.0A HK1168867A1 (en) | 2010-10-14 | 2012-09-28 | Natural adhesive using garlic and method of fabricating the same |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104786721A (en) * | 2015-04-30 | 2015-07-22 | 王振环 | Method for manufacturing sheet material for engraving prints |
| CN106188317A (en) * | 2016-07-13 | 2016-12-07 | 广西梧州市明阳生化科技有限公司 | A kind of enzyme reaction stabilizing buffer and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5647465A (en) * | 1979-09-27 | 1981-04-30 | Dainippon Pharmaceut Co Ltd | Industrial paste consisting of tamarind seed powder solubilized in cold water |
| FR2730236A1 (en) * | 1995-02-08 | 1996-08-09 | Generale Sucriere Sa | Utilising sugar beet pulp after extn. of saccharose |
-
2010
- 2010-10-14 CN CN 201010509499 patent/CN102443363B/en not_active Expired - Fee Related
-
2012
- 2012-09-28 HK HK12109658.0A patent/HK1168867A1/en not_active IP Right Cessation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5647465A (en) * | 1979-09-27 | 1981-04-30 | Dainippon Pharmaceut Co Ltd | Industrial paste consisting of tamarind seed powder solubilized in cold water |
| FR2730236A1 (en) * | 1995-02-08 | 1996-08-09 | Generale Sucriere Sa | Utilising sugar beet pulp after extn. of saccharose |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104786721A (en) * | 2015-04-30 | 2015-07-22 | 王振环 | Method for manufacturing sheet material for engraving prints |
| CN104786721B (en) * | 2015-04-30 | 2017-07-21 | 江俞 | A kind of preparation method of etching |
| CN106188317A (en) * | 2016-07-13 | 2016-12-07 | 广西梧州市明阳生化科技有限公司 | A kind of enzyme reaction stabilizing buffer and application thereof |
| CN106188317B (en) * | 2016-07-13 | 2019-01-25 | 广西梧州市明阳生化科技有限公司 | A kind of enzyme reaction stabilizing buffer and its application |
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| HK1168867A1 (en) | 2013-01-11 |
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