CN104177627B - A kind of natural lacquer tree fat emulsion with bacteriostatic activity and preparation method thereof - Google Patents

A kind of natural lacquer tree fat emulsion with bacteriostatic activity and preparation method thereof Download PDF

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CN104177627B
CN104177627B CN201410402086.0A CN201410402086A CN104177627B CN 104177627 B CN104177627 B CN 104177627B CN 201410402086 A CN201410402086 A CN 201410402086A CN 104177627 B CN104177627 B CN 104177627B
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tree fat
lacquer tree
preparation
fat emulsion
emulsion
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CN104177627A (en
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王成章
陈虹霞
周昊
叶建中
陶冉
张宇思
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Nanjing Zhongsen Biotechnology Co., Ltd.
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Institute of Chemical Industry of Forest Products of CAF
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Abstract

The invention discloses a kind of natural lacquer tree fat emulsion with bacteriostatic activity and preparation method thereof, it is made up of lacquer tree fat, nonionic surfactant, cationic surfactant, co-emulsifier, pH value regulator, antioxidant and water, by lacquer tree fat, surfactant and help Emulsion first carry out fusing stirring, it is slow added into deionized water and is stirred emulsifying, generate emulsion oil-in-water.The emulsion prepared has good bin stability, dewatering ability, dilution stability and bacteriostasis property, can be widely applied to industry and the fields such as preserving fruit and vegetable utilizing, material waterproofing, cosmetics, leather.Production technology of the present invention is easily executed and raw material natural environmental-protective, and suitable large-scale promotion uses.

Description

A kind of natural lacquer tree fat emulsion with bacteriostatic activity and preparation method thereof
Technical field
The present invention relates to, with the Vegetable oil lipoprotein lacquer tree fat of natural reproducible as raw material, may be used for the preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity in the fields such as material waterproofing, preserving fruit and vegetable utilizing, cosmetics.
Background technology
Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) refers mainly to Anacardiaceae, a class plant of paint genus (Toxicodendron), it it is one of traditional economic forest of China, its cultivation history is long, variety source enriches, it is referred to as state's paint or lacquer because a kind of lacquer (i.e. Resina Toxicodendri verniciflui) of secretion has the Optimality of uniqueness, enjoys great prestige both at home and abroad.The fruit of Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) is also known as paint seed, and in flat the most spherical, annual 9 ~ October of autumn is ripe.Peel divides 3 layers, outer peel film quality;Mesocarp is wax coat, can extract lacquer tree fat, for light yellow or celadon;Kernel is seed, can squeeze urushoil.Lacquer tree fat chemical composition by 90%~95% triglyceride, 3%~15% free fatty, 1%~2% free alkyl alcohol form, wherein conjugated fatty acid by 70%~75% Palmic acid, 3%~5% stearic acid, 15%~35% oleic acid, 2%~5% binary of fatty acids form.Because it has the dicarboxylic acid component of uniqueness, give and paint higher elasticity and pliability, there is the unexistent smooth texture of general vegetable wax and glutinous toughness.
Existing more than the 100 year history of the wild lacquer tree fat of Japan's processing, in numerous production fields, utilization rate is high, such as waterproofing agent, coating, bonding agent, the food demoulding, add lustre to and pack and fruit freshness preserving etc., especially in the cosmetics of super quality, electrofax toner, textile printing and dyeing material and the masking of electronic chip, medicine there is effect unique on soft or hard cream, Emulsion and surgical bandage.China is shorter to the processing and utilization time of lacquer tree fat, and the research to lacquer tree fat at present the most still concentrates on the aspects such as its chemical composition, physical and chemical performance and decolorizing and refining processing technique.Wax emulsion is with a wide range of applications, and can be applicable to the fields such as agricultural, papermaking, weaving, wood-based plate, leather, automobile, pottery, rubber and building.In recent years, along with people's reinforcement to environmental consciousness, natural emulsion is increasingly favored by people, applies in gardens especially as fruit and vegetable fresh-keeping agent, water-retaining agent, the aspect such as fruit and vegerable, family property.
Existing Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) colony of China has more than 30 kind, produces paint seed amount about more than 150 ten thousand tons per year, rank first in the world, but these affluent resources the most do not obtain high-valued utilization.The present invention utilizes this natural reproducible resource of lacquer tree fat, and exploitation has the lacquer tree fat emulsion of excellent dewatering ability, dilution stability and storage-stable, is formed and a kind of has good film-forming property, homogeneous, the stable natural emulsion having no side effect.By the application of the present invention, can further widen the range of application of lacquer tree fat, improve the comprehensive benefit of lacquer tree resource.
Summary of the invention
In order to promote to paint the higher value application of seed resource, also for the raw material sources of the emulsifing wax widening natural green further, some problems solving the existence of present stage lacquer tree fat application aspect provide a kind of natural lacquer tree fat emulsion with bacteriostatic activity and preparation method thereof.
For realizing object above, the present invention carries out emulsifying with lacquer tree fat, nonionic surfactant, cationic surfactant, co-emulsifier, pH value regulator, antioxidant and water composition, concretely comprises the following steps:
(1) it is the lacquer tree fat of 10-20% by percentage by weight, the nonionic surfactant of 10-20%, 2-8% cationic surfactant and 0.3-2% co-emulsifier are placed in equipped with in the reaction vessel of reflux, being heated to 60-100 DEG C makes it melt, open stirring, control rotating speed at 500-2500rpm/min, make material mix homogeneously, add the deionized water of 48-77% and the antioxidant of 0.5-1%, stirring, emulsifying phase inversion, emulsifying 40-120min, add 0.2-0.5%pH value regulator, make pH value between 6.5-7, obtain lacquer tree fat emulsion, its solid content is 20-33%, viscosity is 10-70 mPas, dewatering ability, bin stability and dilution stability are 1 grade;Lacquer tree fat emulsion concentration is that 0.1 ~ 1mg/mL has, to staphylococcus aureus, escherichia coli, bacillus subtilis, Bacillus cereus, bacillus pyocyaneus and Klebsiella pneumonia, the effect of significantly inhibiting, and its inhibition zone meansigma methods is 2.1 ~ 2.8cm;
(2) one or more in polysorbate60, Tween 80, Span 80, tea saponin, Gleditschiasaponin, sapindoside and sucrose ester of nonionic surfactant in this patent.One or more in methanol, ethanol, glycerol, n-butyl alcohol of co-emulsifier.Cationic surfactant is the quaternary ammonium salt surface active agent with bacteriostasis.One or more in ammonia, triethylamine, dimethyl amine, dimethylethanolamine of pH value regulator.One or more in vitamin C, vitamin E and gallic acid of antioxidant.
Beneficial effect:
The present invention is with lacquer tree fat in paint seed as raw material, preparing natural lacquer tree fat emulsion, the product prepared has good emulsion property and bacteriostasis property, and sample source Nantural non-toxic side effect, biological degradable, at aspects such as material water conservation, preserving fruit and vegetable utilizing and cosmetics, there is good application prospect;
The present invention has not only widened the raw material sources of natural emulsion, expands the purposes of paint seed the most further, and the higher value application for Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) entirety resource provides a kind of approach.
Accompanying drawing explanation
The microscope scanning figure of Fig. 1 lacquer tree fat (a) and lacquer tree fat dilute emulsion (b).
Detailed description of the invention
Following example are some citings of the present invention, should not be seen as limitation of the invention.
The preparation of embodiment 1 lacquer tree fat emulsion
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, by nonionic surfactant 10-20g, cationic surfactant 2-8g with help Emulsion 0.3-2g to add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the antioxidant of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5gpH value regulator, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
The selection of embodiment 2 different emulsifiers
The emulsifying agent using different HLB value carries out the preparation of O/W type emulsion.Select polysorbate60, Tween 80, Span 80, tea saponin, Gleditschiasaponin, sapindoside, sucrose ester and quaternary ammonium salt surface active agent to carry out emulsification experiment, from dewatering ability, bin stability and dilution stability Integrated comparative, the results are shown in Table 1.As can be seen from the table, composite emulsifier has excellent dewatering ability, dilution stability and bin stability.
The impact on emulsion property of the table 1 different emulsifiers type.
Embodiment 3
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, 4 emulsifying agent 10-20g, quaternary ammonium salt surface active agent 2-8g will be compounded and methanol 0.3-2g will add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the Vc of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5g ammonia, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
Embodiment 4
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, 5 emulsifying agent 10-20g, quaternary ammonium salt surface active agent 2-8g will be compounded and ethanol 0.3-2g will add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the Ve of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5g triethylamine, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
Embodiment 5
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, 6 emulsifying agent 10-20g, quaternary ammonium salt surface active agent 2-8g will be compounded and glycerol 0.3-2g will add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the gallic acid of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5g triethylamine, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
Embodiment 6
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, 7 emulsifying agent 10-20g, quaternary ammonium salt surface active agent 2-8g will be compounded and n-butyl alcohol 0.3-2g will add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the Vc of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5g dimethyl amine, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
Embodiment 7
Refined lacquer tree fat 10-20g is added in the there-necked flask equipped with agitator thermometer, stirring is warmed up to 60-100 DEG C, after it dissolves, 6 emulsifying agent 10-20g, quaternary ammonium salt surface active agent 2-8g will be compounded and ethanol 0.3-2g will add in oil phase, stir, in reaction vessel, add the deionized water of 48-77g, add in two times, ON cycle water;Add water for the first time, stirring (controlling rotating speed 500-2500rpm/min) emulsifying, prepare water-in-oil type lacquer tree fat colostrum;Then the water of surplus and the Vc of 0.5-1g are added, stirring, emulsifying phase inversion, continues emulsifying 40-120min, adds 0.2-0.5g dimethylethanolamine, make pH value between 6.5-7, obtain lacquer tree fat emulsion.
Embodiment 8 response surface design optimization
With emulsifier (X1), mixing speed (X2) and emulsification times (X3) as independent variable, viscosity (Y1) and dewatering ability (Y3) are response value, carry out response surface design analysis, and experimental result is shown in Table 2.As can be seen from the table, along with the increase of emulsifier, viscosity presents the trend of increase, and dewatering ability reaches 1 grade the most therewith.Along with the increase of mixing speed, viscosity increases along with the increase of mixing speed, and dewatering ability reaches 1 grade the most therewith, occurs slightly downward trend afterwards.Along with the prolongation of emulsification times, viscosity and dewatering ability gradually tend to mild, the time, each of emulsion reached optimal to performance after 80 min.
Table 2 lacquer tree fat dilute emulsion response surface design result of the test.
To response value Y1(i.e. viscosity in table 6) carry out polynary quadratic regression equation, Y2=51.83+16.59X1+5.8X2+8.31X3+0.53X1X2-1.31X1X3+4.97X2X3-0.84X12-10.72X22-8.23X32.Model is carried out variance analysis and significance test, and result is as shown in table 3.From table 3 it can be seen that the F of model returns=6.64, P=0.0104 < 0.05, show that the secondary model that experiment is used is significant, the most meaningful.Lose and intend item P=0.8105 > 0.05, be favourable to model, exist without losing pseudo-factor, therefore can replace experiment true point that experimental result is analyzed with this regression equation.The primary and secondary that factor affects is may determine that by the size of regression equation first order absolute value.In optimizing technique, the factor size affecting emulsion viscosity is emulsifier > emulsification times > mixing speed.
The variance analysis of the regression model of table 7 response value viscosity.
The optimum process condition being calculated lacquer tree fat dilute emulsion by above-mentioned regression model is: emulsifier is 18%, mixing speed is 1800 rpm, emulsification times is 100 min, lacquer tree fat consumption is 10%, temperature 80 DEG C, emulsifying agent is composite emulsifier 4-7 type, and now its emulsion viscosity is 69.2 mPa.s, solid content is 32.2%, and dewatering ability is 1 grade.Carrying out replication experiment by above-mentioned process conditions, parallel 3 times, the emulsion viscosity obtained is 71.5mPa.s, and solid content is 33%, and dewatering ability is 1 grade, and storage-stable is 1 grade.
Embodiment 9
Fig. 1 is lacquer tree fat and lacquer tree fat dilute emulsion amplifies the scanning figure after 400 times, it can be seen that lacquer tree fat raw material is more viscous, in bulk in microscope.Lacquer tree fat dilute emulsion is the least granule, and ratio is more uniform, illustrates that lacquer tree fat sufficiently scatter in emulsion.
Embodiment 10
Natural lacquer tree fat emulsion and methyl hydroxybenzoate are configured to 2.0g/mL sample solution, preparation staphylococcus aureus, escherichia coli, bacillus subtilis, Bacillus cereus, bacillus pyocyaneus and the bacteria suspension of Klebsiella pneumonia, choose 106Cfu/mL is filter paper enzyme coating concentration.The results are shown in Table 4.As can be seen from the table, natural lacquer tree fat emulsion is suitable with the bacteriostasis of methyl hydroxybenzoate.
The bacteriostasis of different strain is compared by table 4 natural lacquer tree fat emulsion and methyl hydroxybenzoate.

Claims (7)

1. having a preparation method for the natural lacquer tree fat emulsion of bacteriostatic activity, it includes the component of following weight proportioning:
Lacquer tree fat 10-20%
Nonionic surfactant 10-20%
Cationic surfactant 2-8%
Co-emulsifier 0.3-2%
PH value regulator 0.2-0.5%
Antioxidant 0.5-1.5%
Distilled water 48-77%.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that comprise the steps:
It is the lacquer tree fat of 10-20% by percentage by weight, the nonionic surfactant of 10-20%, 2-8% cationic surfactant and 0.3-2% co-emulsifier are placed in equipped with in the reaction vessel of reflux, being heated to 60-100 DEG C makes it melt, open stirring, control rotating speed at 500-2500rpm, make material mix homogeneously, add the distilled water of 48-77% and the antioxidant of 0.5-1%, stirring, emulsifying phase inversion, emulsifying 40-120min, add 0.2-0.5%pH value regulator, make pH value between 6.5-7, obtain lacquer tree fat emulsion, its solid content is 20-33%, viscosity is 10-70 mPa s, dewatering ability, bin stability and dilution stability are 1 grade;Lacquer tree fat emulsion concentration is that 0.1 ~ 1mg/mL has, to staphylococcus aureus, escherichia coli, bacillus subtilis, Bacillus cereus, bacillus pyocyaneus and Klebsiella pneumonia, the effect of significantly inhibiting, and its inhibition zone meansigma methods is 2.1 ~ 2.8cm.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that one or more in polysorbate60, Tween 80, Span 80, tea saponin, Gleditschiasaponin, sapindoside and sucrose ester of nonionic surfactant.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that one or more in methanol, ethanol, glycerol, n-butyl alcohol of co-emulsifier.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that cationic surfactant is quaternary ammonium salt surface active agent.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that one or more in ammonia, triethylamine, dimethyl amine, dimethylethanolamine of pH value regulator.
The preparation method of a kind of natural lacquer tree fat emulsion with bacteriostatic activity, it is characterised in that one or more in vitamin C, vitamin E and gallic acid of antioxidant.
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CN105613721A (en) * 2015-12-29 2016-06-01 江苏省农业科学院 Preservative and preparation method and application thereof
CN106165720A (en) * 2016-07-01 2016-11-30 江苏省农业科学院 1 MCP combines the compounding preservation method of lacquer tree fat
CN108395546A (en) * 2017-02-06 2018-08-14 上海诺科生物科技有限公司 A kind of ester type waxes lotion and preparation method thereof
CN108935968A (en) * 2018-07-26 2018-12-07 中国林业科学研究院林产化学工业研究所 A kind of feeding fatty powder of water soluble coating aliphatic radical and preparation method thereof
CN116144415A (en) * 2022-12-28 2023-05-23 刘艳平 Composite modified emulsified lubricating oil

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CN103666279A (en) * 2012-09-24 2014-03-26 天津博克尼科技发展有限公司 Anti-static vehicle paint surface body polishing emulsion wax

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