CN107699392B - Preparation method of beer bottle sterilization cleaning agent based on microcrystalline cellulose/silver composite material - Google Patents
Preparation method of beer bottle sterilization cleaning agent based on microcrystalline cellulose/silver composite material Download PDFInfo
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- CN107699392B CN107699392B CN201710830665.9A CN201710830665A CN107699392B CN 107699392 B CN107699392 B CN 107699392B CN 201710830665 A CN201710830665 A CN 201710830665A CN 107699392 B CN107699392 B CN 107699392B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/83—Mixtures of non-ionic with anionic compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
- C11D3/1206—Water-insoluble compounds free metals, e.g. aluminium grit or flakes
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/37—Polymers
- C11D3/3703—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C11D3/373—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicones
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/662—Carbohydrates or derivatives
Abstract
The invention discloses a preparation method of a beer bottle sterilization cleaning agent based on a microcrystalline cellulose/silver composite material. The beer bottle sterilization cleaning agent prepared by the invention has the advantages of strong detergency, good anti-fouling redeposition capability, easiness in rinsing to remove fouling, good cleaning effect on the fouling of beer bottles, capability of reducing equipment fouling, contribution to smooth operation of a system, capability of synchronously completing sterilization and disinfection on the beer bottles, good sterilization effect and capability of effectively improving the sanitary performance of the cleaned beer bottles.
Description
Technical Field
The invention relates to the technical field of cleaning agents, and particularly relates to a preparation method of a beer bottle sterilization cleaning agent based on a microcrystalline cellulose/silver composite material.
Background
With the increasing production of beer, many enterprises begin to use recycled beer bottles in order to save production cost. In order not to affect the inherent quality of beer products, the cleaning of beer bottles is a key process for recycling beer bottles. The dirt composition of beer bottles is quite complex, and mainly comprises dust, grease, protein, wine dirt, colloid, mildew stains, adhesive and the like. The prior beer bottle cleaning agent is mainly compounded by alkali, surfactant and other components, has poor anti-redeposition capacity of a system, and mainly has the following defects:
1. after being peeled off, the dirt is secondarily attached to the beer bottle body due to the high settling speed, so that the cleaning capability of the dirt is influenced, and the equipment is easy to scale.
2. The cleaning agent has single performance, can only remove dirt and clean, cannot eliminate the adverse effect of bacteria and mould breeding in the beer bottle on the sanitation of the beer bottle, and the sanitation of the cleaned beer bottle is poor.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a preparation method of a beer bottle sterilization cleaning agent with good anti-fouling redeposition capability and strong killing performance. The nano silver is permeated into the inner space of the interweaved cellulose crystal to enable the cellulose crystal to have antibacterial performance; the nano microcrystalline cellulose treated by the enzyme method has the property of loose and porous surface, and is more favorable for adsorbing dirt, bacteria and the like; the secondary attachment of dirt is reduced by adding the sophorose lactone biological non-toxic non-ionic surfactant.
The invention also aims to provide a preparation method of the beer bottle sterilization cleanser based on the microcrystalline cellulose/silver composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material comprises the following steps:
(1) firstly, adding microcrystalline cellulose into a sodium citrate buffer solution to be uniformly dispersed to obtain microcrystalline cellulose suspension, then adding a certain amount of cellulase to carry out enzymolysis reaction at 50-60 ℃ for 24-48h, and carrying out centrifugal separation to obtain nano microcrystalline cellulose suspension;
(2) mixing the nano microcrystalline cellulose suspension and a silver nitrate solution according to the volume ratio (1-2): (0.5-1) uniformly mixing to obtain a mixed solution, then adding the mixed solution and deionized water with the volume 20-30 times of that of the mixed solution into a reaction kettle to react for 1-2h at the temperature of 120-130 ℃, and cooling to obtain nano-silver-loaded nano microcrystalline cellulose suspension;
(3) firstly, 0.3-0.5 part by weight of sodium hydroxide, 0.1-0.15 part by weight of sodium carbonate, 0.3-0.5 part by weight of sodium dodecyl sulfate, 0.3-0.5 part by weight of sophorose lactone and 0.03-0.05 part by weight of dimethyl silicone oil are uniformly mixed, then 80-100 parts by weight of nano-silver loaded nano microcrystalline cellulose suspension is added and uniformly mixed, and the beer bottle sterilizing cleaning agent is obtained.
The technical requirements for preparing the raw materials of the invention are as follows: the pH value of the sodium citrate buffer solution is 4.4-4.8, and the concentration is 0.03-0.05 mol/L; the solid content of the microcrystalline cellulose suspension is 1-1.5%; the adding amount of the cellulase is that 10-15U cellulase is added into every gram of microcrystalline cellulose; the mass fraction of the silver nitrate solution is 1-1.5%.
The using method comprises the following steps: when cleaning beer bottles, the disinfectant is diluted by 1:52-83 times and then used, and the beer bottles need to be fully watered after use.
Compared with the prior art, the invention has the following beneficial effects:
the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material has the advantages that the formula is adjusted, so that the product has better dirt removing capability, and meanwhile, the sterilization effect is good, and the specific effects are as follows:
(1) the nano microcrystalline cellulose loaded with nano silver is prepared by mixing nano microcrystalline cellulose prepared by an enzyme method as a reducing agent with silver nitrate and then performing a hydrothermal synthesis reaction by utilizing the property that the surface of the microcrystalline cellulose has a large number of reducing end groups, and the sterilization of coliform and staphylococcus aureus can reach 5 log values under the use condition.
(2) The nano microcrystalline cellulose treated by the enzyme method has loose and porous surface, is more favorable for adsorbing dirt, bacteria and the like, and can effectively prevent the dirt from redepositing due to the unique suspension dispersing capacity. By adding the solubilizing, emulsifying, wetting, foaming, dispersing, surface tension reducing and other performances of the nontoxic biological non-surfactant sophorose lactone, the beer bottle sterilization cleaning agent prepared by the invention has the advantages of strong detergency, good anti-dirt redeposition capability, easy rinsing for removing dirt, good cleaning effect on the dirt of beer bottles, and obviously higher cleaning effect on the dirt containing carbon and nitrogen than the commercial alkaline wine bottle cleaning agent.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to these examples, and any modification made without departing from the spirit of the present invention falls within the scope of the present invention.
The preparation method of the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material comprises the following steps:
(1) firstly, adding microcrystalline cellulose into a sodium citrate buffer solution to be uniformly dispersed to obtain microcrystalline cellulose suspension, then adding a certain amount of cellulase to carry out enzymolysis reaction at 50-60 ℃ for 24-48h, and carrying out centrifugal separation to obtain nano microcrystalline cellulose suspension;
(2) uniformly mixing the nano microcrystalline cellulose suspension and a silver nitrate solution according to a volume ratio of (1-2): 0.5-1) to obtain a mixed solution, then adding the mixed solution and deionized water which is 20-30 times of the volume of the mixed solution into a reaction kettle to react for 1-2h at the temperature of 120 ℃ and 130 ℃, and cooling to obtain nano silver-loaded nano microcrystalline cellulose suspension;
(3) firstly, 0.3-0.5 part by weight of sodium hydroxide, 0.1-0.15 part by weight of sodium carbonate, 0.3-0.5 part by weight of sodium dodecyl sulfate, 0.3-0.5 part by weight of sophorose lactone and 0.03-0.05 part by weight of dimethyl silicone oil are uniformly mixed, then 80-100 parts by weight of nano-silver loaded nano microcrystalline cellulose suspension is added and uniformly mixed, and the beer bottle sterilizing cleaning agent is obtained.
The pH value of the sodium citrate buffer solution is 4.4-4.8, and the concentration is 0.03-0.05 mol/L.
The solid content of the microcrystalline cellulose suspension is 1-1.5%.
The adding amount of the cellulase is that 10-15U of cellulase is added into every gram of microcrystalline cellulose.
The mass fraction of the silver nitrate solution is 1-1.5%.
Example 1:
the preparation method of the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material comprises the following steps:
(1) firstly, adding microcrystalline cellulose into a sodium citrate buffer solution to be uniformly dispersed to obtain microcrystalline cellulose suspension, then adding a certain amount of cellulase to carry out enzymolysis reaction at 50 ℃ for 24 hours, and carrying out centrifugal separation to obtain nano microcrystalline cellulose suspension;
(2) mixing the nano microcrystalline cellulose suspension and a silver nitrate solution according to the volume ratio of 1: 0.5, uniformly mixing to obtain a mixed solution, adding the mixed solution and deionized water with the volume 20 times that of the mixed solution into a reaction kettle together, reacting for 1h at 120 ℃, and cooling to obtain nano silver-loaded nano microcrystalline cellulose suspension;
(3) firstly, 0.3 part by weight of sodium hydroxide, 0.1 part by weight of sodium carbonate, 0.3 part by weight of sodium dodecyl sulfate, 0.3 part by weight of sophorose lactone and 0.03 part by weight of dimethyl silicone oil are mixed uniformly, and then 80 parts by weight of nano-silver loaded nano microcrystalline cellulose suspension is added and mixed uniformly to obtain the beer bottle sterilization cleaning agent.
The pH value of the sodium citrate buffer solution is 4.8, and the concentration is 0.05 mol/L.
The microcrystalline cellulose suspension has a solid content of 1%.
The adding amount of the cellulase is that 10U of cellulase is added into each gram of microcrystalline cellulose.
The mass fraction of the silver nitrate solution is 1%.
Example 2:
the preparation method of the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material comprises the following steps:
(1) firstly, adding microcrystalline cellulose into a sodium citrate buffer solution to be uniformly dispersed to obtain microcrystalline cellulose suspension, then adding a certain amount of cellulase to carry out enzymolysis reaction at 60 ℃ for 24 hours, and carrying out centrifugal separation to obtain nano microcrystalline cellulose suspension;
(2) uniformly mixing the nano microcrystalline cellulose suspension and a silver nitrate solution according to the volume ratio of 2:1 to obtain a mixed solution, adding the mixed solution and deionized water which is 27 times of the volume of the mixed solution into a reaction kettle to react for 2 hours at 124 ℃, and cooling to obtain nano silver-loaded nano microcrystalline cellulose suspension;
(3) firstly, 0.5 part by weight of sodium hydroxide, 0.15 part by weight of sodium carbonate, 0.3 part by weight of sodium dodecyl sulfate, 0.3 part by weight of sophorose lactone and 0.03 part by weight of dimethyl silicone oil are mixed uniformly, and then 100 parts by weight of nano-silver loaded nano microcrystalline cellulose suspension is added and mixed uniformly to obtain the beer bottle sterilization cleaning agent.
The pH value of the sodium citrate buffer solution is 4.6, and the concentration is 0.05 mol/L.
The microcrystalline cellulose suspension had a solid content of 1.2%.
The adding amount of the cellulase is 12U cellulase added into each gram of microcrystalline cellulose.
The mass fraction of the silver nitrate solution is 1.2%.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
And (5) testing the corrosion of the metal.
First, equipment
1. Metal sheet: copper sheet, carbon steel sheet, poster sheet and stainless steel sheet
2. Analytical balance: BA110S 30904575
3. And (3) sterilizing and cleaning agent: beer bottle sterilization cleaning agent based on microcrystalline cellulose/silver composite material
Second, method
1. The inspection basis is as follows: ministry of health, Disinfection Specification (2002 edition) 2.2.4 determination of Metal corrosivity
2. And (3) testing conditions: ambient temperature 21 ℃ and relative humidity 50%.
3. The test concentrations were dilutions (1:52) in the range of the concentrations used.
Three, result in
Degree of corrosion of metal by disinfectant
Fourth, conclusion
A1: 52 diluent of the microcrystalline cellulose/silver composite material-based beer bottle sterilization cleaning agent moderately corrodes carbon steel sheets, copper sheets and aluminum sheets and slightly corrodes stainless steel.
Quantitative colibacillus killing experiment
First, equipment
1. Test strains: escherichia coli (8099) (5 th-7 th generation)
2. A disinfectant: beer bottle sterilization cleaning agent based on microcrystalline cellulose/silver composite material
3. Neutralizing agent: solution of 0.5% sodium thiosulfate, 1% tween-80, 0.5% lecithin
4. Sterile hard water
5. Diluting liquid: (TPS)
Second, method
1. The inspection basis is as follows: the second part of the Disinfection product inspection Specification of the Ministry of health (2002 edition), 2.1.1.5.5 neutralizer identification test, 2.1.1.7.4 quantitative bacteria killing test.
2. And (3) identification test of a neutralizer: diluting solution at a ratio of 1:83, acting for 3.5min, and testing temperature: the 20 ℃ test was repeated 3 times. 3. And (3) sterilization test: 1:83 dilution, test temperature: the 20 ℃ test was repeated 3 times.
Three, result in
1. Neutralizer identification test
(1) The error rate between groups 3, 4 and 5 was 4.21%.
(2) The serial numbers and contents of the groups listed in the table are the same as the specifications of the inspection bases.
TABLE 1 neutralizing agent test identification results
2. Killing effect on test bacteria
TABLE 2 Effect on Escherichia coli
Note: negative control sterile growth
Fourth, conclusion
Beer bottle bactericidal detergent 1 based on microcrystalline cellulose/silver composite: 83 when diluted, the neutralizing agent containing 0.5 percent of sodium thiosulfate, 1 percent of Tween-80 and 0.5 percent of lecithin can effectively neutralize the action of the neutralizing agent on the tested bacteria remained on the surface of the escherichia coli, and the neutralizing agent and a neutralized product have no adverse effect on the tested bacteria and a culture medium.
2. After 3 repeated tests, based on microcrystalline cellulose/silver composite material, the beer bottle sterilization cleaning agent 1:83 when diluted, the average killing logarithm value of the colibacillus is more than or equal to 5.00 when the colibacillus is acted for 3.5 min.
Quantitative killing experiment for staphylococcus aureus
First, equipment
1. Test strains: staphylococcus aureus (ATCC6538) (3 rd-5 th generation)
2. A disinfectant: beer bottle sterilization cleaning agent based on microcrystalline cellulose/silver composite material
3. Neutralizing agent: solution of 0.5% sodium thiosulfate, 1% tween-80, 0.5% lecithin
4. Sterile hard water
5. Diluting liquid: (TPS)
Second, method
1. The inspection basis is as follows: disinfection product inspection technical Specification section II Disinfection technical Specification of the Ministry of health (2002 edition), 2.1.1.7.4 bacteria quantitative kill test.
2. And (3) sterilization test: 1:83 dilution, test temperature: the 20 ℃ test was repeated 3 times.
Three, result in
Killing effect on staphylococcus aureus
Note: negative control sterile growth
Fourth, conclusion
After 3 repeated tests, based on microcrystalline cellulose/silver composite material, the beer bottle sterilization cleaning agent 1:83 when diluted, the average killing logarithm value of the staphylococcus aureus after 3.5min of action is more than or equal to 5.00.
Experiment for removing dirt
1. Organic carbon content comparison: respectively putting the treated beer bottles with dirt into a commercially available alkaline wine bottle cleaning agent
Cleaning with microcrystalline cellulose/silver composite material in sterilizing detergent for 5min, and dissolving in water respectively before and after cleaning
The organic carbon content was determined after diluting the solution 3mL by 1000 times.
Comparison of carbon cleaning content
2. Organic nitrogen content comparison: respectively putting the treated beer bottles with dirt into a commercially available alkaline wine bottle cleaning agent
And cleaning with microcrystalline cellulose/silver composite material in sterilizing detergent for 5min, respectively dissolving
The solution was 10mL, and the organic nitrogen content was measured.
Content comparison after organic Nitrogen cleaning
And (4) conclusion:
the composite material beer bottle sterilizing detergent has obviously higher cleaning effect on dirt containing carbon and nitrogen than the commercial alkaline wine bottle detergent.
Claims (1)
1. The preparation method of the beer bottle sterilization cleaning agent based on the microcrystalline cellulose/silver composite material is characterized by comprising the following steps:
(1) firstly, adding microcrystalline cellulose into a sodium citrate buffer solution to be uniformly dispersed to obtain microcrystalline cellulose suspension, then adding a certain amount of cellulase to carry out enzymolysis reaction at 50-60 ℃ for 24-48h, and carrying out centrifugal separation to obtain nano microcrystalline cellulose suspension;
(2) uniformly mixing the nano microcrystalline cellulose suspension and a silver nitrate solution according to a volume ratio of (1-2): 0.5-1) to obtain a mixed solution, then adding the mixed solution and deionized water which is 20-30 times of the volume of the mixed solution into a reaction kettle to react for 1-2h at the temperature of 120 ℃ and 130 ℃, and cooling to obtain nano silver-loaded nano microcrystalline cellulose suspension;
(3) firstly, 0.3-0.5 part by weight of sodium hydroxide, 0.1-0.15 part by weight of sodium carbonate, 0.3-0.5 part by weight of sodium dodecyl sulfate, 0.3-0.5 part by weight of sophorose lactone and 0.03-0.05 part by weight of dimethyl silicone oil are uniformly mixed, and then 80-100 parts by weight of nano-silver loaded nano microcrystalline cellulose suspension is added and uniformly mixed to obtain the beer bottle sterilizing and cleaning agent;
the pH value of the sodium citrate buffer solution is 4.4-4.8, and the concentration is 0.03-0.05 mol/L;
the solid content of the microcrystalline cellulose suspension is 1-1.5%;
the adding amount of the cellulase is that 10-15U cellulase is added into every gram of microcrystalline cellulose;
the mass fraction of the silver nitrate solution is 1-1.5%.
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