CN102559418B - Phytic acid silver toilet soap and preparation method thereof - Google Patents

Phytic acid silver toilet soap and preparation method thereof Download PDF

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CN102559418B
CN102559418B CN 201210004001 CN201210004001A CN102559418B CN 102559418 B CN102559418 B CN 102559418B CN 201210004001 CN201210004001 CN 201210004001 CN 201210004001 A CN201210004001 A CN 201210004001A CN 102559418 B CN102559418 B CN 102559418B
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phytic acid
acid silver
silver
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CN102559418A (en
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雷学军
祝加铧
雷谨榕
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雷学军
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Abstract

The invention relates to the field of toilet soap and provides phytic acid silver toilet soap and a preparation method thereof. The phytic acid silver toilet soap comprises phytic acid silver, wherein the phytic acid silver accounts for 0.01 to 0.5 percent of the mass of the toilet soap. The preparation method for the phytic acid silver toile soap comprises the following steps: hydrolyzing palm oil under the action of sodium hydroxide to generate sodium carboxylate solution, crushing phytic acid silver precipitate, adding the powder into the sodium carboxylate solution and reacting, wherein the pH value is adjusted to be 8 to 9 by citric acid monohydrate; and dehydrating, drying, adding essence and performing compression molding. The phytic acid silver toilet soap has a good effect of killing bacteria, viruses, fungi and other pathogenic microorganisms.

Description

A kind of phytic acid silver perfumed soap and preparation method thereof
Technical field
The present invention relates to the perfumed soap field, be specifically related to a kind of phytic acid silver perfumed soap and preparation method thereof.
Background technology
Silver ions has remarkable sterilization and disinfection effect.General microbiotic on average can only play effect to 6 kinds of germs, but silver ions can be eliminated 650 kinds of germs.Silver ions can slacken the activity of germ body endo enzyme, thereby can prevent the patience reinforcement of side effect and germ, fundamentally controls the breeding of germ.Ag+ can adsorb the sulfydryl on the proteolytic enzyme in the bacterial body consumingly and (SH), combine with it rapidly, make the proteolytic enzyme loss of activity, cause bacterium death.After bacterium was killed by Ag+, Ag+ dissociated out again from the bacterium corpse, contacted with other bacterium colony again, carried out said process again and again, and this also is the lasting reason of silver-colored germicidal action.According to surveying and determination, when containing Ag+ in the water and being 0.01mg/L, just can kill the intestinal bacteria in the water fully, can keep reaching and not multiply the flora that makes new advances in 90 days.Perfumed soap sterilizing ability in the market a little less than, do not have the perfumed soap of broad-spectrum antimicrobial, do not have phytic acid silver perfumed soap yet.
Summary of the invention
The technical problem to be solved in the present invention is at the weak point of existing perfumed soap, to have proposed a kind of phytic acid silver perfumed soap and preparation method thereof.Phytic acid silver perfumed soap fusing point of the present invention is low, particle is thin, relative density is little, sterilizing ability is strong, is difficult for by skin absorption, to the skin nonirritant, and is nontoxic to human body.
Technical scheme of the present invention is:
A kind of phytic acid silver perfumed soap comprise phytic acid silver, and the mass content of phytic acid silver in perfumed soap is 0.01%~0.5%.
Phytic acid silver of the present invention prepares by the following method: add solid nitric acid silver in the volumetric molar concentration of phytic acid radical ion is 6%~10% plant acid solution, make that the mol ratio of silver ions and phytic acid radical ion is 0.3~1: 1, adopting Citric acid monohydrate Food grade to regulate pH is 8~10, and temperature maintenance was stirred 1.8~2.2 hours down at 80 ℃~95 ℃; Concentrate, be cooled to 3 ℃~7 ℃ then, add anhydrous propanone, obtain the precipitation of phytic acid silver, the add-on of anhydrous propanone is 0.9~1.1 times of solution quality after concentrating.
Phytic acid silver of the present invention preferably prepares by the following method: add solid nitric acid silver in the volumetric molar concentration of phytic acid radical ion is 10% plant acid solution, make that the mol ratio of silver ions and phytic acid radical ion is 1: 1, adopting Citric acid monohydrate Food grade to regulate pH is 10, and temperature maintenance was stirred 2 o'clock down at 95 ℃; Concentrate, be cooled to 5 ℃ then, add anhydrous propanone, obtain the precipitation of phytic acid silver, the add-on of anhydrous propanone is 1 times of solution quality after concentrating.
The preparation method of a kind of phytic acid silver perfumed soap of the present invention may further comprise the steps:
(1) plam oil hydrolysis generation mass concentration under the effect of sodium hydroxide is 30%~40% carboxylic acid sodium solution;
(2) phytic acid silver precipitation being pulverized the back crosses to add in the above-mentioned carboxylic acid sodium solution behind 280~320 mesh sieves and reacts, wherein phytic acid silver is 0.01~0.2: 1 with the mass ratio of carboxylic acid sodium solution, temperature control adopts Citric acid monohydrate Food grade to regulate between pH to 8~9 at 25 ℃~70 ℃;
(3) dewatering, be dried to water content is 10%~30%;
(4) dried object adds essence compression moulding by 180~220 purpose screen filtrations, gets final product.
Below the present invention will be further explained and the explanation:
The reaction of preparation phytic acid silver perfumed soap is as follows:
C 6H 18O 24P 6+AgNO 3→Ag 12C 6H 6O 24P 6+HNO 3
RCOONa+Ag 12C 6H 6O 24P 6→RCOOAg
One, the preparation method of phytic acid silver is as follows, referring to Fig. 1:
1, be to add solid nitric acid silver in 6~10% the plant acid solution in phytic acid concentration, make that the mol ratio of silver ions and phytic acid radical ion is 0.3~1: 1, adopting Citric acid monohydrate Food grade to regulate pH is 8~10, and temperature maintenance was stirred 1.8~2.2 hours down at 80 ℃-95 ℃;
Salt-forming reaction is:
Figure BDA0000129212750000031
2, after salt-forming reaction finishes, reaction solution is concentrated 4 hours.
3, concentrated solution is cooled to 5 ± 2 ℃, preferably is 1: 1 ratio adding anhydrous propanone in solution quality ratio after concentrating, and precipitation is separated out.
4, precipitation is dehydrated, just obtain crystalloid phytic acid silver.
Two, the preparation method of phytic acid silver perfumed soap is as follows, referring to Fig. 2:
1, plam oil hydrolysis under the effect of sodium hydroxide generates carboxylate salt.
Saponification reaction is: RCOOR+NaOH → RCOONa+ROH
Plam oil is to the skin gentleness, and cleaning power is strong; Oleic acid content is 40%, and the power of preserving moisture is strong; INS value 145.All can carry out saponification reaction between 25-70 ℃, temperature is carried out the saponification reaction best results at 50 ℃.
2, after 300 mesh sieves are crossed in the broken back of phytic acid silver powder, add in the RCOONa solution.
Replacement(metathesis)reaction is: RCOONa+Ag 12C 6H 6O 24P 6→ RCOOAg
Phytic acid silver is 0.01~0.2: 1 with the mass ratio of carboxylic acid sodium solution, and temperature is controlled at 25-70 ℃, adopts Citric acid monohydrate Food grade to be adjusted between pH8~9.
3, after replacement(metathesis)reaction finishes, reaction solution dehydration 2 hours.
4, the object after the dehydration is dried to moisture water gaging 10~30%.
5, dried object adds essence compression moulding by 180~220 purpose screen filtrations, gets final product.
Compared with prior art, advantage of the present invention is:
1, the method for preparing phytic acid silver perfumed soap of the present invention is simple, and temperature of reaction is low, and product, color and luster is good, purity is high, stability is high.
2, product of the present invention is a kind of daily skin surface sanitary product, and is easy to use, and multiple germ is had the ability of killing.
3, the invention provides a kind of novel disinfecting type phytic acid silver perfumed soap, silver ions in the perfumed soap reaches 100% to the killing rate of intestinal bacteria, streptococcus aureus, Candida albicans bacterium, can effectively kill poliomyelitis virus I-type in the water, can also effectively remove pseudopodium protozoon in the water, contain yellow pigment protozoon, actinomycetes etc.
Description of drawings
Fig. 1 is preparation technology's schema of phytic acid silver;
Fig. 2 is phytic acid silver perfumed soap preparation technology schema.
Embodiment
The present invention will be further explained and explanation below in conjunction with specific embodiment:
Embodiment 1:
Referring to Fig. 1, described phytic acid silvery is equipped with technology:
1, in concentration is 6~10% plant acid solution, adds Silver Nitrate, adopt Citric acid monohydrate Food grade to be adjusted between PH8~10, stirred 2 hours; Use thermostat, with temperature maintenance at 80~95 ℃.
Salt-forming reaction is:
2, after salt-forming reaction finishes, reaction solution is concentrated 4 hours.
3, concentrated solution is cooled to 5 ± 2 ℃, adds anhydrous propanone, and the add-on of anhydrous propanone is 0.9~1.1 times of solution quality after concentrating, and precipitation is separated out.
4, precipitation is dehydrated, just obtain crystalloid phytic acid silver.
Table 1 phytic acid silvery is equipped with the experiment contrast
First group Second group The 3rd group
Phytic acid concentration 6% 8% 10%
PH value 8 9 10
Temperature 80℃ 90℃ 95℃
Salify speed Slow fast Generally Best
As can be seen from Table 1, phytic acid silvery is equipped with in the process, and phytic acid concentration is 10%, PH10, and during 95 ℃ of temperature, reaction better.
Embodiment 2:
Referring to Fig. 2, phytic acid silver perfumed soap preparation technology:
1, plam oil hydrolysis under the effect of sodium hydroxide generates carboxylic acid sodium, obtains mass concentration and be 35% carboxylic acid sodium solution.
Saponification reaction is: RCOOR+NaOH → RCOONa+ROH
Plam oil is to the skin gentleness, and cleaning power is strong; Oleic acid content is 40%, and the power of preserving moisture is strong; INS value 145.All can carry out saponification reaction between 25~70 ℃, temperature is carried out the saponification reaction best results at 50 ℃.
2, with behind broken back 300 mesh sieves excessively of the phytic acid silver powder of the 3rd group of preparation of embodiment 1, add in the RCOONa solution and react;
Replacement(metathesis)reaction is: RCOONa+Ag 12C 6N 6O 24P 6→ RCOOAg
Phytic acid silver is 0.01~0.2: 1 with the mass ratio of carboxylic acid sodium solution, and temperature is controlled at 25~70 ℃, adopts Citric acid monohydrate Food grade to be adjusted between PH8~9.
3, after replacement(metathesis)reaction finishes, reaction solution dehydration 2 hours.
4, to be dried to water content be 25% to the object after the dehydration.
5, dried object adds essence compression moulding by 200 purpose screen filtrations.
The contrast of table 2 phytic acid silver perfumed soap preparation experiment
Figure BDA0000129212750000061
As can be seen from Table 2, in the preparation of phytic acid silver perfumed soap, phytic acid silver is 0.2: 1 with the mass ratio of carboxylic acid sodium solution, and 70 ℃ of temperature during pH value 9, are reacted the fastest.By finished product the test of Bacillus subtilus killing effect and finished product are tested as can be known the intestinal bacteria killing effect, phytic acid silver perfumed soap has sterilising effect preferably, but when the content of phytic acid silver in the phytic acid silver perfumed soap was higher, corresponding cost also increased to some extent.

Claims (3)

1. a phytic acid silver perfumed soap is characterized in that, comprise phytic acid silver, and the mass content of phytic acid silver in perfumed soap is 0.01%~0.5%;
Described phytic acid silver prepares by the following method: add solid nitric acid silver in the volumetric molar concentration of phytic acid radical ion is 6%~10% plant acid solution, make that the mol ratio of silver ions and phytic acid radical ion is 0.3~1:1, adopting Citric acid monohydrate Food grade to regulate pH is 8~10, and temperature maintenance was stirred 1.8~2.2 hours down at 80 ℃~95 ℃; Concentrate, be cooled to 3 ℃~7 ℃ then, add anhydrous propanone, obtain the precipitation of phytic acid silver, the add-on of anhydrous propanone is 0.9~1.1 times of solution quality after concentrating;
Described phytic acid silver perfumed soap is prepared by following method:
(1) plam oil hydrolysis generation mass concentration under the effect of sodium hydroxide is 30%~40% carboxylic acid sodium solution;
(2) after crossing 280~320 mesh sieves after the pulverizing of phytic acid silver precipitation, add mixing in the above-mentioned carboxylic acid sodium solution, wherein phytic acid silver is 0.01~0.2:1 with the mass ratio of carboxylic acid sodium solution, temperature control adopts Citric acid monohydrate Food grade to regulate between pH to 8~9 at 25 ℃~70 ℃;
(3) dewatering, be dried to water content is 10%~30%;
(4) dried object adds essence compression moulding by 180~220 purpose screen filtrations, gets final product.
2. according to the described phytic acid silver of claim 1 perfumed soap, it is characterized in that, described phytic acid silver prepares by the following method: add solid nitric acid silver in the volumetric molar concentration of phytic acid radical ion is 10% plant acid solution, make that the mol ratio of silver ions and phytic acid radical ion is 1:1, adopting Citric acid monohydrate Food grade to regulate pH is 10, and temperature maintenance was stirred 2 hours down at 95 ℃; Concentrate, be cooled to 5 ℃ then, add anhydrous propanone, obtain the precipitation of phytic acid silver, the add-on of anhydrous propanone is 1 times of solution quality after concentrating.
3. the preparation method of the described a kind of phytic acid silver perfumed soap of one of claim 1-2 is characterized in that, may further comprise the steps:
(1) plam oil hydrolysis generation mass concentration under the effect of sodium hydroxide is 30%~40% carboxylic acid sodium solution;
(2) after crossing 280~320 mesh sieves after the pulverizing of phytic acid silver precipitation, add mixing in the above-mentioned carboxylic acid sodium solution, wherein phytic acid silver is 0.01~0.2:1 with the mass ratio of carboxylic acid sodium solution, temperature control adopts Citric acid monohydrate Food grade to regulate between pH to 8~9 at 25 ℃~70 ℃;
(3) dewatering, be dried to water content is 10%~30%;
(4) dried object adds essence compression moulding by 180~220 purpose screen filtrations, gets final product.
CN 201210004001 2012-01-06 2012-01-06 Phytic acid silver toilet soap and preparation method thereof Expired - Fee Related CN102559418B (en)

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WO2014170187A1 (en) * 2013-04-16 2014-10-23 Unilever Plc Soap bar having enhanced antibacterial activity
MX2016009881A (en) * 2014-01-29 2016-10-28 Unilever Nv Cleansing compositions containing stable silver.

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1064279A (en) * 1991-02-23 1992-09-09 雷学军 Technology for producing series products of phytate
CN1141162A (en) * 1995-10-20 1997-01-29 江门市蓬江区伟达日用化工厂 Method for producing underarm odour removing agent "Yexiangling"

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1064279A (en) * 1991-02-23 1992-09-09 雷学军 Technology for producing series products of phytate
CN1141162A (en) * 1995-10-20 1997-01-29 江门市蓬江区伟达日用化工厂 Method for producing underarm odour removing agent "Yexiangling"

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