CN114517133B - Microemulsion fruit and vegetable detergent - Google Patents

Microemulsion fruit and vegetable detergent Download PDF

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Publication number
CN114517133B
CN114517133B CN202011290713.8A CN202011290713A CN114517133B CN 114517133 B CN114517133 B CN 114517133B CN 202011290713 A CN202011290713 A CN 202011290713A CN 114517133 B CN114517133 B CN 114517133B
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water
fruit
microemulsion
phase
limonene
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CN114517133A (en
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柳滢春
熊文明
黄勇
肖丽凤
陈冬泳
童宇
何秋华
彭烛
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Zhongshan Torch Polytechnic
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Zhongshan Torch Polytechnic
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/825Mixtures of compounds all of which are non-ionic
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/12Water-insoluble compounds
    • C11D3/1233Carbonates, e.g. calcite or dolomite
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/2075Carboxylic acids-salts thereof
    • C11D3/2079Monocarboxylic acids-salts thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/221Mono, di- or trisaccharides or derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/38Products with no well-defined composition, e.g. natural products
    • C11D3/384Animal products
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/48Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Inorganic Chemistry (AREA)
  • Molecular Biology (AREA)
  • Zoology (AREA)
  • Detergent Compositions (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a microemulsion fruit and vegetable detergent, which comprises the following components in percentage by mass: 9-15% of limonene, 6-10% of alkyl glucoside, 5-9% of coconut oil derivative, 3-7% of sucrose fatty acid ester, 0.5-1% of micro-nano shell powder, a proper amount of auxiliary agent and water. The product of the invention is stable and safe, has excellent double cleaning performances of physical adsorption removal and chemical dissolution removal for dirt, pesticide residue and heavy metal on the surfaces of fruits and vegetables, and also has sterilization and bacteriostasis effects.

Description

Microemulsion fruit and vegetable detergent
[ field of technology ]
The invention relates to a microemulsion fruit and vegetable detergent, belonging to the technical field of daily chemical products.
[ background Art ]
With the progress of society and the increase of people's attention to health, vegetables and fruits have taken an increasingly important role in people's diet structure, and fresh vegetables and fruits are important sources of essential exogenous nutrients such as vitamins, minerals and dietary fibers necessary for people's daily life. In order to ensure the yield of fruits and vegetables, farmers often apply a lot of pesticides, and the heavy metal enrichment of the fruits and vegetables is increased due to pollution of water sources and soil. The problem of pesticide residue and excessive heavy metal on vegetables and fruits causes concern for more and more consumers. After the human body eats fruits and vegetables containing pesticides or heavy metal ions exceeding the standard, toxic substances accumulate in the human body for a long time to cause various chronic diseases, and more troublesome is that some pesticide residues have genetic toxicity. To address this problem, many consumers choose a fruit and vegetable cleaning agent to clean the fruit and vegetable. Various fruit and vegetable cleaning products appear in the market, and fruit and vegetable detergent is a mainstream product, but because a lot of products have lower technical content, if only a few artificial synthetic surfactants are added with auxiliary agents to be simply compounded, the selected petrochemical raw materials are not safe enough, and the fruit and vegetable detergent has no obvious effect on pesticide removal effect after use, has serious problems such as secondary pollution and the like, and has potential safety hazard. The research and development of natural raw materials for preparing efficient and safe fruit and vegetable detergent has become a folk problem to be solved urgently.
[ invention ]
The invention aims to overcome the defects of the prior art and provide the microemulsion fruit and vegetable detergent which has good pesticide residue removing effect and stable and safe system.
The invention adopts the following technical scheme to realize the aim:
the micro-emulsion fruit and vegetable detergent is characterized by comprising the following components in percentage by mass:
the invention relates to a microemulsion fruit and vegetable detergent which is characterized by further comprising the following components in percentage by mass:
0.5 to 1 percent of micro-nano shell powder
Proper amount of auxiliary agent
Water was added to 100%.
In the invention, the auxiliary agent comprises one or more of glycerol, pH regulator, essence and preservative.
The invention relates to a microemulsion fruit and vegetable detergent, which is prepared by the following steps:
a. uniformly mixing limonene, alkyl glucoside, coconut oil derivatives, sucrose fatty acid ester and corresponding water, and heating to 65-75 ℃ to dissolve and transparent to form a transparent microemulsion phase;
b. pre-dissolving preservative and/or essence and part of water;
c. heating glycerin, micro-nano shell components and the balance of water to 80-90 ℃ under stirring to dissolve and transparent to form a water phase, and preserving heat;
d. slowly adding the water phase prepared in the step c into the three-phase micro-emulsion limonene phase prepared in the step a, emulsifying, homogenizing, adding a pH regulator to regulate the pH value, cooling to 45 ℃, adding a pre-dissolved preservative and/or essence, uniformly stirring, cooling and discharging.
The microemulsion technology is a system which is prepared by a certain technological method through an oil phase, a water phase, a surfactant and a cosurfactant phase and has the emulsion particle size of 10-100nm, and the microemulsion system has ultralow interfacial tension, large solubilization capacity, small particle size and excellent thermodynamic stability, and can improve the capability of dissolving pesticides to remove pesticides to a large extent.
Limonene, which is widely found in natural plant peel, is generally extracted from discarded citrus peel. Limonene can be used as an antioxidant and a preservative in food additives, is a natural excellent surfactant in the field of daily chemicals, and has good fat-dissolving and decontamination capability. Limonene has good antibacterial activity, has the potential of becoming a natural preservative, has good biodegradability and does not cause any pollution to the environment.
The micro-nano shell powder is powder obtained by crushing shells through micro-nano, wherein 95% of the main components of the micro-nano shell powder are calcium carbonate, and a small amount of amino acid and polysaccharide substances. The porous fibrous double helix structure has the effects of adsorption and decomposition. In addition, the shell powder has strong antibacterial and bactericidal effects on escherichia coli. The harmful components have antiseptic function.
The invention prepares a three-phase microemulsion limonene system by using plant-source surfactant, cosurfactant, plant-source grease limonene, water and other raw materials through a microemulsion technology. As the emulsion grain size of the microemulsion fruit and vegetable detergent is smaller than that of the general detergent, the microemulsion fruit and vegetable detergent can interact with pesticides and heavy metals on fruits and vegetables more fully and can be dissolved and removed from the fruits and vegetables.
Compared with the prior art, the invention has the following advantages:
the product of the invention is stable and safe, has excellent double cleaning performances of physical adsorption removal and chemical dissolution removal for dirt, pesticide residue and heavy metal on the surfaces of fruits and vegetables, and also has sterilization and bacteriostasis effects.
[ detailed description ] of the invention
The invention is described in further detail below in connection with specific examples:
the invention discloses a microemulsion fruit and vegetable detergent, which comprises the following components in percentage by mass:
the three-phase microemulsion limonene system (three-phase microemulsion limonene phase) was optimized as follows, and the specific orthogonal table design is shown in table 1.
Table 1: mass ratio of each component of three-phase microemulsion limonene phase
The results of the orthogonal test are shown in Table 2, and the results of the analysis of variance are shown in Table 3.
Table 2: orthogonal test design and results
TABLE 3 orthogonal test analysis of variance table
Note that: * P <0.1
In test nos. 1 to 9, the particle size of the prepared three-phase microemulsion limonene system is the smallest under the main raw material proportion of test No. 3, and the proportion is A 1 B 3 C 3 D 3 Namely, the mass ratio of limonene, alkyl glucoside, coconut oil derivative and sucrose fatty acid ester is 9:10:9:7, the particle size of the obtained three-phase microemulsion limonene system is 59.7nm. The average value results corresponding to the usage conditions of each component in Table 2 are as follows: when the mass ratio of limonene, alkyl glucoside, coconut oil derivative and sucrose fatty acid ester is 12, 10, 9 and 7, the average value of the particle diameters of the corresponding microemulsions is the smallest, namely A 2 B 3 C 3 D 3 . Therefore, experiments are carried out under the condition, and the particle size of the obtained three-phase micro-emulsion limonene system is 60.1nm. Considering that the cleaning ability of a three-phase microemulsion limonene system is important, in addition to particle size, the amount of limonene is also an important factor. Under the same conditions, the content of limonene is increased, and the cleaning capability is enhanced. Considering two important factors determining the cleaning capacity of the system, namely limonene and particle size, the optimal dosage is selected as follows: the dosage ratio of limonene, alkyl glucoside, coconut oil derivative and sucrose fatty acid ester is 12, 10, 9 and 7.
The primary and secondary order of analyzing the influence of the consumption of 4 raw materials on the particle size of the prepared three-phase micro-emulsion limonene system micro-emulsion according to the extremely poor results in table 2 is as follows: b > A > D > C, show that C has small influence on the particle size of the prepared three-phase microemulsion limonene system microemulsion, so C is selected as an error column of orthogonal test variance analysis. From the analysis of variance results table 3, it is known that a and B have significant meanings under the condition of a=0.1, and on the other hand, a and B play a decisive role in the formation of the microemulsion, and the particle size of the microemulsion becomes significantly smaller under the action of a and B. However, C, D has no significant effect on the particle size of the three-phase microemulsion limonene system, because the two are mainly auxiliary effects and do not play a decisive role in the system.
In the process production, the raw material saving is significant because both A and B have significance, the important factors of the cleaning capability of the system are comprehensively considered by comprehensively considering the limonene and the particle size, and the C, D influence on the particle size of the three-phase microemulsion limonene system is not significant, thereby keeping A 2 、B 3 On the premise of the raw material condition, the raw material consumption of C, D is reduced, the possibility of the scheme is verified by test number 6 in the orthogonal test result, and the method is characterized in that 2 B 3 C 1 D 2 The particle size of the obtained three-phase microemulsion system is 60.4nm under the coordination of the raw materials. In order to save the cost of raw materials, the finally determined optimization process scheme of the test is as follows: a is that 2 B 3 C 1 D 2
Comparison verification test:
to compare three optimized dosage ratio systems A of limonene, alkyl glucosides, coconut oil derivatives, sucrose fatty acid esters analyzed by orthogonal experiments 1 B 3 C 3 D 3 (example 1), A 2 B 3 C 3 D 3 (example 2), A 2 B 3 C 1 D 2 (example 3) practical effect on pesticide removal to obtain the optimal comprehensive technological scheme referring to the method for testing the pesticide removal rate in GB/T24691-2009 fruit and vegetable cleaning agent, the test pesticide is selected from typical representative cypermethrin, each group is tested 3 times, and the average value is obtained. The test results of the three-phase microemulsion limonene system are shown in table 4:
table 4: comparing the test results
From the test results, three preferable usage rates of the three-phase microemulsion limonene system are ranked as follows compared with the removal rate of typical pesticide cypermethrin: a is that 2 B 3 C 3 D 3 >A 2 B 3 C 1 D 2 >A 1 B 3 C 3 D 3 92.0%, 91.5% and 90.1% respectively. The reason for this is analyzed, the effect of the three-phase microemulsion limonene system on removing pesticide residues is closely related to the particle size of the microemulsion, and the particle sizes of the three preferred systems are respectively 60.1nm, 60.4nm and 59.7nm, which are related to the dosage of four main raw material components, especially the dosage of the raw material A, B. Comparative A 1 B 3 C 3 D 3 ,A 2 B 3 C 3 D 3 A is a 2 B 3 C 1 D 2 The amount of limonene, the main cleaning power component of both preferred systems, is significantly increased. And in the aspect of the particle size of the formed microemulsion, compared with the component C, D, A, B, the particle size of the three-phase microemulsion limonene system microemulsion is more obviously influenced. Therefore A 2 B 3 C 3 D 3 A is a 2 B 3 C 1 D 2 The pesticide residue removal rate of the two preferred systems is higher. And for A 2 B 3 C 3 D 3 A is a 2 B 3 C 1 D 2 Two preferred systems, the microemulsion particle size is less different, and A 2 B 3 C 3 D 3 Although the dosage of C, D is obviously higher than that of A 2 B 3 C 1 D 2 The method has the advantages that the pesticide residue removal rate is not obvious, the factors such as resource conservation, product cost and the like are comprehensively considered, and the finally determined comprehensive optimization process scheme is as follows: a is that 2 B 3 C 1 D 2
The micro-emulsion fruit and vegetable detergent also comprises the following components in parts by mass:
0.5 to 1 percent of micro-nano shell powder
Proper amount of auxiliary agent
Water was added to 100%.
The application examples of the microemulsion fruit and vegetable detergent of the invention are shown in Table 5.
Table 5: the mass percentage of each component is 5 percent
The preparation method of examples 1-3 is:
a. heating the phase A to 80-90 ℃ under stirring to dissolve and transparent to form a water phase, and preserving heat;
b. pre-dissolving the phase C;
c. uniformly mixing the phase B, and heating to 65-75 ℃ to dissolve and transparent to form a three-phase micro-emulsion limonene phase;
d. slowly adding phase A into phase B, emulsifying, homogenizing, adding pH regulator to regulate pH value, cooling to 45deg.C, adding pre-dissolved phase C, stirring, cooling, and discharging.
Evaluation of the fruit and vegetable detergent products of examples 1 to 3.
1. The fruit and vegetable detergent is evaluated for stability, appearance and smell according to the row standard, and the centrifugal stability tests of the fruit and vegetable detergent of examples 1-3 are all stable without layering, and the appearance is thick liquid and has lemon fragrance.
2. Physical and chemical indexes of the fruit and vegetable detergent of examples 1-3 are shown in Table 6.
Table 6:
3. the microbial detection results of the fruit and vegetable detergents of examples 1-3 show that the bacterial count is less than 10CFU/g and the coliform group is less than 3MPN/100g.
4. Foaming property measurement: in the rogowski foam meter, 3:1000 a ratio of 500ml of the fruit and vegetable detergent products of examples 1-3 were diluted and the resulting foam volume was measured after flowing from a height of 450mm to the liquid surface of the same solution. The test procedure was carried out according to the national standard GB/T7462-94, and the results were measured 30s, 3min and 5min after stopping the liquid flow, and the foam heights of examples 1-3 were all greater than 18.4mm,15.5mm and 10.8mm, with good foaming ability.
5. Pesticide residue removing effect of fruit and vegetable detergent product
The pesticide residue removal effect of the fruit and vegetable detergent is roughly tested by using the pesticide residue test card, and the results are shown in Table 7. As shown by rough measurement, the fruit and vegetable detergents in examples 1-3 have good pesticide residue removal effect and good removal effect as the result that the removal effect of two commercially available fruit and vegetable cleaning agents is in C.
Table 7: test result of pesticide residue removal effect test card
Remarks: a: white represents the pesticide residue content range: 7-9
B: light blue indicates that the pesticide residue content ranges are: 4-6
C: blue represents the pesticide residue content range: 0-3
The pesticide residue removal precision test experiments of the examples 1-3 and the commercially available fruit and vegetable detergents 1 and 2 are carried out, and the pesticide removal rate test method in the GB/T24691-2009 fruit and vegetable cleaning agent is referred to, wherein the typical representative cypermethrin and propoxur are selected as the test pesticides, and each group of tests is carried out for 3 times, and the average value is obtained. Tests show that the removal rate of the cypermethrin in the examples 1-3 reaches more than 95%, the removal rate of the propoxur reaches more than 99%, and the propoxur is superior to two commercially available fruit and vegetable detergents.
Compared with the common fruit and vegetable cleaning agent, the three-phase microemulsion system of the fruit and vegetable detergent enhances the dissolving and removing functions of the fruit and vegetable detergent on pesticide residues, and simultaneously has the dual functions of physical adsorption and removal and chemical dissolving and removal on the pesticide residues.

Claims (1)

1. The micro-emulsion fruit and vegetable detergent is characterized by comprising the following components in percentage by mass:
limonene 9-15%
6 to 10 percent of alkyl glucoside
Coconut oil derivative 5-9%
Sucrose fatty acid ester 3-7%
45 to 55 percent of water
0.5 to 1 percent of micro-nano shell powder
Proper amount of auxiliary agent
Water was added to 100%,
the auxiliary agents are glycerol, a pH regulator, essence and a preservative;
the microemulsion fruit and vegetable detergent is prepared by the following method:
a. uniformly mixing limonene, alkyl glucoside, coconut oil derivatives, sucrose fatty acid ester and corresponding water, and heating to 65-75 ℃ to dissolve and transparent to form a microemulsion phase;
b. pre-dissolving preservative, essence and part of water;
c. heating glycerin, micro-nano shell powder and the balance of water to 80-90 ℃ under stirring to dissolve and transparent to form a water phase, and preserving heat;
d. slowly adding the water phase prepared in the step c into the three-phase micro-emulsion limonene phase prepared in the step a, emulsifying, homogenizing, adding a pH regulator to regulate the pH value, cooling to 45 ℃, adding a pre-dissolved preservative and/or essence, uniformly stirring, cooling and discharging;
the corresponding water in the step a is 45-55% of water in the components.
CN202011290713.8A 2020-11-18 2020-11-18 Microemulsion fruit and vegetable detergent Active CN114517133B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104388208A (en) * 2014-11-07 2015-03-04 舟山赛莱特海洋科技有限公司 Method for preparing pesticide-removing fruit and vegetable cleaning agent based on shell powder
CN106544163A (en) * 2015-09-16 2017-03-29 周国萍 A kind of fruit and vegerable special cleaning
CN108865490A (en) * 2018-07-18 2018-11-23 苏州绿叶日用品有限公司 The fruits and vegetables cleaning agent and preparation method thereof of microemulsion dosage removal pesticide residue
JP2020050782A (en) * 2018-09-27 2020-04-02 株式会社Adeka Liquid detergent composition

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104388208A (en) * 2014-11-07 2015-03-04 舟山赛莱特海洋科技有限公司 Method for preparing pesticide-removing fruit and vegetable cleaning agent based on shell powder
CN106544163A (en) * 2015-09-16 2017-03-29 周国萍 A kind of fruit and vegerable special cleaning
CN108865490A (en) * 2018-07-18 2018-11-23 苏州绿叶日用品有限公司 The fruits and vegetables cleaning agent and preparation method thereof of microemulsion dosage removal pesticide residue
JP2020050782A (en) * 2018-09-27 2020-04-02 株式会社Adeka Liquid detergent composition

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