CN103555225B - A kind of preparation method of Silver ion anti-bacterial glue - Google Patents
A kind of preparation method of Silver ion anti-bacterial glue Download PDFInfo
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- CN103555225B CN103555225B CN201310471265.5A CN201310471265A CN103555225B CN 103555225 B CN103555225 B CN 103555225B CN 201310471265 A CN201310471265 A CN 201310471265A CN 103555225 B CN103555225 B CN 103555225B
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Abstract
The invention belongs to chemical technology field, the invention discloses a kind of preparation method of Silver ion anti-bacterial glue, the present invention with the short lint cellulose of natural phant for main raw material, in the basic conditions through hydroxypropylation, methylate after the Vltra tears that generates again through water-soluble high-molecular compound that silver ions-Vltra tears is repeatedly wrapped to form; Again through the soluble substance such as polyvinyl alcohol, redispersable latex powder, with to be dry mixed or wet-mix method makes Silver ion anti-bacterial glue; Preparation method's advantage of Silver ion anti-bacterial glue of the present invention is that ecological silver ions has the effect of permanent fungus and mildew resistance, and this product is easy to use again, is powder preparation, avoids the problem such as recruitment, transport, pollution that secondary glue brings; Really accomplish low-carbon energy-saving, environmental protection, and Silver ion anti-bacterial glue prepared by the present invention has sterilizing ability by force, the advantage that sterilization effect is lasting.
Description
Technical field
The present invention relates to technical field of chemistry and chemical engineering, particularly relate to a kind of preparation method of Silver ion anti-bacterial glue.
Background technology
Silver ions, we can be regarded as a kind of anti-biotic material or material, the anti-microbial effect of material, the detrimentally affect and consequence that produce at the vitality of certain material to microorganism in general, these detrimentally affects and consequence, the most concentrated performance is exactly affect microbial growth, breeding so that death.Namely suppress microbial growth, breed or kill the effect of microorganism.Relation between anti-biotic material and microorganism can regard the relation of microorganism and environment as, and particularly to the virose environment of microorganism, the silver ion antimicrobial agent mechanism of action has the following aspects.
1, the synthesis of interference cell wall.Bacteria cell wall important component is peptidoglycan, and silver ion antimicrobial agent, to the interference effect of cell walls, main suppresses that polysaccharide chain and tetrapeptide are crosslinked link, thus makes cell walls lose integrity, loses the provide protection to osmotic pressure, damages thalline and dead.
2, can damaging cells film.Cytolemma is the important integral part of bacterial cell vital movement.Therefore, as damaged membrane wound, destroy, will bacterial death be caused.
3, the synthesis of arrestin matter.The building-up process of protein changes, stops, making bacterial death.
4, the synthesis of interfere RNA.Be in a word hinder copying of genetic information, comprise the synthesis of DNA, RNA, and DNA profiling transcript mRNA etc.
Because silver has adsorption to the microorganism in liquid, after microorganism is adsorbed by silver, play respiratory enzyme and just lose effect, microorganism will be dead rapidly.The sterilizing ability of silver ions is strong especially, as long as containing the silver ions of 2/1sts milligrams in every premium on currency, can kill most of bacterium in water.The U.S. one scientist once did overtesting, and by 4.5 liters of sewage (every milliliter containing intestinal bacteria more than 7,000), after the silver electrode process of 3 hours, all intestinal bacteria are all dead for he.Typhoid fever bacterium can only live 18 hours on silver strip, and diphtheria bacterium can only live 3 days on silver strip.
Sterilizing ability just because of silver is very strong, again to people and animals without any injury, at present, the airline exceeding half has in the world used the water strainer of silvery.The swimming pool of many countries also purifies with silver, and the water after purification can not as using the water of pharmaceutical chemicals purification, and stimulate eyes and the skin of swimmer, silver ion antimicrobial agent is also applied on weaving face fabric.
Current silver ions is also widely applied in the paint series products such as emulsion paint, reach the effect of sterilization, mildew-resistant, but mostly antibacterial effect is poor for silver ion glue series products in the market, can only solve and cover epidermis, the sterilization on surface, mildew-proof function; The substantive sterilization of interior substrate, mildew-resistant and permanent sterilization, anti-mold effect can not be solved.
Summary of the invention
For solve existing silver ion glue series products mostly antibacterial effect poor, can not the shortcoming of profound sterilization and persistence sterilization, the present invention proposes a kind of preparation method of Silver ion anti-bacterial glue.
The present invention adopts following technical scheme:
The preparation method of Silver ion anti-bacterial glue of the present invention comprises the following steps:
(1) preparation of silver ions Vltra tears; In reactor, add velveteen, and then in reactor, add the sodium hydroxide solution that mass concentration is 50%, reactor is evacuated down to-0.09 ~-0.1MPa, with nitrogen replacement 3 times; Then in reactor, propylene oxide is added;
(2) mixed solution passing into dme, methyl chloride and propylene oxide is 0.6 ~ 1.8MPa to reactor pressure, stirring at room temperature 0.5 ~ 2.0h;
(3) pass into the mixed solution of dme, methyl chloride and propylene oxide, maintenance reactor pressure is 0.6 ~ 1.8MPa, when 60-65 DEG C, and reaction 2-3h; At 70-90 DEG C, reaction 1 ~ 4h;
(4) extent of reaction in detection reaction device, when the methyl content of reaction product Vltra tears be greater than 20.2%, hydroxypropyl content be greater than 6.0% time, stopped reaction;
(5) reclaim unreacted methyl chloride and dme solvent, add the hot water of more than 90 DEG C simultaneously;
(6) in reactor, add hydrochloric acid, adjust ph is to 7.5-7.8;
(7) in reactor, add 10% silver nitrate solution, be uniformly mixed 30min;
(8) by mixture centrifuge dewatering in reactor, then solid materials uses hot wash 1-2 time of more than 90 DEG C;
(9) finally carry out drying, silver-ion antibiotic Vltra tears can be obtained.
(10) make: the material by following weight part:
Polyvinyl alcohol 30-60
Redispersable latex powder 10-30
Plant bean gum 3-5
Sodium alginate, thickening material 0.1-0.5
Silver-ion antibiotic Vltra tears 30-50; To drop in rotary agitator mixing kettle dry blending 30-50 minute homogeneous, packing successively and get final product.
In step (1), velveteen is the short velveteen of Powdered natural phant, and particle diameter is 60-120 order.
In step (1), the mass ratio of velveteen and sodium hydroxide solution is 1:0.5 ~ 1:1.
In step (1), the add-on of velveteen and the mass ratio of propylene oxide are 1:0.2 ~ 1:0.6.
In step (2), (3), the volume ratio of the mixed solution of dme, methyl chloride and propylene oxide consists of: 52% dme, 43% methyl chloride and 5% propylene oxide.
In step (2), (3), reactor pressure is 0.6 ~ 1.8MPa.
In step (3), temperature of reaction is divided into two stages, first stage: 60-65 DEG C, subordinate phase 70-90 DEG C.
In step (7), the quality of velveteen and the add-on of 10% silver nitrate solution are than being 1:0.001 ~ 1:0.01.
Positively effect of the present invention is as follows:
Preparation method's advantage of Silver ion anti-bacterial glue of the present invention is that ecological silver ions has the effect of permanent fungus and mildew resistance, the technological method wrapped up with the modern times is combined with vegetable fibre and forms colloid, make lake shape again to whitewash or bottoming basement membrane with base-material, thus solve existing environment friendly mildew resistant glue water problem in the lump; This product is easy to use again, is powder preparation, avoids the problem such as recruitment, transport, pollution that secondary glue brings; Really accomplish low-carbon energy-saving, environmental protection, and Silver ion anti-bacterial glue prepared by the present invention has sterilizing ability by force, the advantage that sterilization effect is lasting.
Embodiment
The following examples describe in further detail of the present invention.
Embodiment 1
(1) in reactor, add 100Kg velveteen, velveteen is 60 orders, and then in reactor, add the sodium hydroxide solution that 50Kg mass concentration is 50%, and reactor is evacuated down to-0.09 ~-0.1MPa, with nitrogen replacement 3 times; Then in reactor, 20Kg propylene oxide is added;
(2) the mixed solution reactor pressure passing into dme, methyl chloride and propylene oxide is 0.6MPa, the volume ratio of the mixed solution of dme, methyl chloride and propylene oxide consists of: 52% dme, 43% methyl chloride and 5% propylene oxide, stirring at room temperature 0.5h;
(3) pass into the mixed solution of dme, methyl chloride and propylene oxide, maintenance reactor pressure is 0.6MPa, 60 DEG C time, and reaction 2h; At 70 DEG C, reaction 1h;
(4) extent of reaction in detection reaction device, when the methyl content of reaction product Vltra tears be greater than 20.2%, hydroxypropyl content be greater than 6.0% time, stopped reaction;
(5) reclaim unreacted methyl chloride and dme solvent, add the hot water of 90 DEG C simultaneously;
(6) in reactor, add hydrochloric acid, adjust ph is to 7.5-7.8;
(7) in reactor, add 10% silver nitrate solution of 0.1Kg, be uniformly mixed 30min;
(8) by mixture centrifuge dewatering in reactor, then solid materials uses hot wash 2-3 time of more than 90 DEG C;
(9) finally carry out drying, packaging can obtain silver-ion antibiotic Vltra tears;
(10) make: the material (Kg) by following weight:
Polyvinyl alcohol 30
Redispersable latex powder 10
Plant bean gum 3
Sodium alginate, thickening material 0.1
Silver-ion antibiotic Vltra tears 30; To drop in rotary agitator mixing kettle dry blending homogeneous, packing in 30 minutes successively and get final product.
Embodiment 2
(1) in reactor, add 100Kg velveteen, velveteen is 120 orders, and then in reactor, add the sodium hydroxide solution that 100Kg mass concentration is 50%, and reactor is evacuated down to-0.09 ~-0.1MPa, with nitrogen replacement 3 times; Then in reactor, 60Kg propylene oxide is added;
(2) mixed solution passing into dme, methyl chloride and propylene oxide is 1.8MPa to reactor pressure, the volume ratio of the mixed solution of dme, methyl chloride and propylene oxide consists of: 52% dme, 43% methyl chloride and 5% propylene oxide, stirring at room temperature 2h;
(3) pass into the mixed solution of dme, methyl chloride and propylene oxide, maintenance reactor pressure is 1.8MPa, 65 DEG C time, and reaction 3h; At 90 DEG C, reaction 4h;
(4) extent of reaction in detection reaction device, when the methyl content of reaction product Vltra tears be greater than 20.2%, hydroxypropyl content be greater than 6.0% time, stopped reaction;
(5) reclaim unreacted methyl chloride and dme solvent, add the hot water of 90 DEG C simultaneously;
(6) in reactor, add hydrochloric acid, adjust ph is to 7.5-7.8;
(7) in reactor, add 10% silver nitrate solution of 1Kg, be uniformly mixed 30min;
(8) by mixture centrifuge dewatering in reactor, then solid materials uses hot wash 2-3 time of more than 90 DEG C;
(9) finally carry out drying, packaging can obtain silver-ion antibiotic Vltra tears;
(10) make: the material (Kg) by following weight:
Polyvinyl alcohol 60
Redispersable latex powder 30
Plant bean gum 5
Sodium alginate, thickening material 0.5
Silver-ion antibiotic Vltra tears 50; To drop in rotary agitator mixing kettle dry blending homogeneous, packing in 50 minutes successively and get final product.
Embodiment 3
(1) in reactor, add 100Kg velveteen, velveteen is 80 orders, and then in reactor, add the sodium hydroxide solution that 80Kg mass concentration is 50%, and reactor is evacuated down to-0.09 ~-0.1MPa, with nitrogen replacement 3 times; Then in reactor, 40Kg propylene oxide is added;
(2) mixed solution passing into dme, methyl chloride and propylene oxide is 1MPa to reactor pressure, the volume ratio of the mixed solution of dme, methyl chloride and propylene oxide consists of: 52% dme, 43% methyl chloride and 5% propylene oxide, stirring at room temperature 0.5h;
(3) pass into the mixed solution of dme, methyl chloride and propylene oxide, maintenance reactor pressure is 1MPa, 60 DEG C time, and reaction 2.5h; At 80 DEG C, reaction 3h;
(4) extent of reaction in detection reaction device, when the methyl content of reaction product Vltra tears be greater than 20.2%, hydroxypropyl content be greater than 6.0% time, stopped reaction;
(5) reclaim unreacted methyl chloride and dme solvent, add the hot water of 90 DEG C simultaneously;
(6) in reactor, add hydrochloric acid, adjust ph is to 7.5-7.8;
(7) in reactor, add 10% silver nitrate solution of 0.5Kg, be uniformly mixed 30min;
(8) by mixture centrifuge dewatering in reactor, then solid materials uses hot wash 2-3 time of more than 90 DEG C;
(9) finally carry out drying, packaging can obtain silver-ion antibiotic Vltra tears;
(10) make: the material (Kg) by following weight:
Polyvinyl alcohol 50
Redispersable latex powder 20
Plant bean gum 4
Sodium alginate, thickening material 0.3
Silver-ion antibiotic Vltra tears 40; To drop in rotary agitator mixing kettle dry blending homogeneous, packing in 40 minutes successively and get final product.
The performance of embodiment 4 silver ion glue
Existing silver ion glue on silver ion glue prepared by embodiment of the present invention 1-3 and market
Be applied in building surface, and carry out sterilization effect mensuration, result is as shown in table 1.
The bactericidal property of silver ion glue prepared by table 1 the present invention
It is strong that the silver ion glue that as can be seen from Table 1 prepared by the present invention has sterilizing ability, the advantage that sterilization effect is lasting.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (7)
1. the preparation method of a Silver ion anti-bacterial glue, it is characterized in that: this preparation method comprises the following steps: the preparation of (1) silver ions Vltra tears: add velveteen in reactor, and then in reactor, add the sodium hydroxide solution that mass concentration is 50%, reactor is evacuated down to-0.09 ~-0.1MPa, with nitrogen replacement 3 times; Then in reactor, propylene oxide is added;
(2) mixed solution passing into dme, methyl chloride and propylene oxide is 0.6 ~ 1.8MPa to reactor pressure, stirring at room temperature 0.5 ~ 2.0h;
(3) pass into the mixed solution of dme, methyl chloride and propylene oxide, maintenance reactor pressure is 0.6 ~ 1.8MPa, when 60-65 DEG C, and reaction 2-3h; At 70-90 DEG C, reaction 1 ~ 4h;
(4) extent of reaction in detection reaction device, when the methyl content of reaction product Vltra tears be greater than 20.2%, hydroxypropyl content be greater than 6.0% time, stopped reaction;
(5) reclaim unreacted methyl chloride and dme solvent, add the hot water of more than 90 DEG C simultaneously;
(6) in reactor, add hydrochloric acid, adjust ph is to 7.5-7.8;
(7) in reactor, add 10% silver nitrate solution, be uniformly mixed 30min;
(8) by mixture centrifuge dewatering in reactor, then solid materials uses hot wash 1-2 time of more than 90 DEG C;
(9) finally carry out drying, silver-ion antibiotic Vltra tears can be obtained;
(10) make: the material by following weight part:
Polyvinyl alcohol 30-60
Redispersable latex powder 10-30
Plant bean gum 3-5
Sodium alginate 0.1-0.5
Silver-ion antibiotic Vltra tears 30-50; To drop in rotary agitator mixing kettle dry blending 30-50 minute homogeneous, packing successively and get final product.
2. preparation method as claimed in claim 1, it is characterized in that: in step (1), velveteen is the short velveteen of Powdered natural phant, and particle diameter is 60-120 order.
3. preparation method as claimed in claim 1, it is characterized in that: in step (1), the mass ratio of velveteen and sodium hydroxide solution is 1:0.5 ~ 1:1.
4. preparation method as claimed in claim 1, it is characterized in that: in step (1), the add-on of velveteen and the mass ratio of propylene oxide are 1:0.2 ~ 1:0.6.
5. preparation method as claimed in claim 1, is characterized in that: in step (2), (3), the volume ratio of the mixed solution of dme, methyl chloride and propylene oxide consists of: 52% dme, 43% methyl chloride and 5% propylene oxide.
6. preparation method as claimed in claim 1, it is characterized in that: in step (2), (3), reactor pressure is 0.6 ~ 1.8MPa.
7. preparation method as claimed in claim 1, is characterized in that: in step (7), and the quality of velveteen and the add-on of 10% silver nitrate solution are than being 1:0.001 ~ 1:0.01.
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| CN103788215A (en) * | 2014-02-19 | 2014-05-14 | 山东光大科技发展有限公司 | Process for producing pharmaceutical auxiliary material hydroxypropyl methylcellulose through slurry process |
| CN103880966B (en) * | 2014-04-11 | 2016-06-01 | 山东赫达股份有限公司 | The preparation method of special Vltra tears is released in slow control |
| CN106065297B (en) * | 2016-08-05 | 2017-11-03 | 宝艺新材料股份有限公司 | A kind of corrugated case with durable antibiotic performance |
| CN110452304A (en) * | 2019-08-20 | 2019-11-15 | 湖州展望天明药业有限公司 | A kind of hydroxypropyl methyl cellulose processing technology |
| CN111519440A (en) * | 2020-04-27 | 2020-08-11 | 江苏笛莎公主文化创意产业有限公司 | Manufacturing process of water printing composite fabric |
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| US20090075007A1 (en) * | 2007-09-13 | 2009-03-19 | 3M Innovative Properties Company | Adhesive composite |
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| CN101058701A (en) * | 2007-05-30 | 2007-10-24 | 陈峰磊 | Water soluble adhesive |
| CN101401586A (en) * | 2008-11-20 | 2009-04-08 | 苏伟 | Simple production method for nano-silver antiseptic solution |
| EP2450389A1 (en) * | 2010-11-08 | 2012-05-09 | EMS-Patent AG | Adhesion promoter for textile reinforcing inserts and their use |
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