CN115644184A - Environment-friendly mildew-removing gel and preparation method thereof - Google Patents

Environment-friendly mildew-removing gel and preparation method thereof Download PDF

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CN115644184A
CN115644184A CN202211172363.4A CN202211172363A CN115644184A CN 115644184 A CN115644184 A CN 115644184A CN 202211172363 A CN202211172363 A CN 202211172363A CN 115644184 A CN115644184 A CN 115644184A
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mildew
parts
stirring
environment
preparation
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唐骏
卓仲标
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Zhejiang Coloray Technology Development Co ltd
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Zhejiang Coloray Technology Development Co ltd
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Abstract

The invention discloses environment-friendly mildew-removing gel and a preparation method thereof, and relates to the technical field of mildew removal. The invention relates to an environment-friendly mildew-removing gel and a preparation method thereof, wherein the environment-friendly mildew-removing gel comprises the following raw materials in parts by weight: 80-100 parts of imazalil, 20-40 parts of glycerol, 10-30 parts of beeswax, 10-20 parts of sodium starch octenyl succinate, 10-20 parts of polycaprolactone and 30-40 parts of mould removing microcapsules, wherein the mould removing microcapsules take a black tea extracting solution as a capsule core, modified cyclodextrin as a capsule shell, and mould removing particles are dispersed in the black tea extracting solution. The invention discloses environment-friendly mildew-removing jelly and a preparation method thereof, wherein the environment-friendly mildew-removing jelly has better adhesion performance through the synergistic effect of all raw materials, can better adhere to the surface of an acting object in the using process, can kill mildew in time, and can achieve the long-acting mildew-removing effect by forming a film layer on the surface of the mildew and combining with mildew-removing microcapsules in the interior.

Description

Environment-friendly mildew-removing gel and preparation method thereof
Technical Field
The invention relates to the technical field of mildew removal, and particularly relates to environment-friendly mildew-removing gel and a preparation method thereof.
Background
The mold is a kind of fungus, and has developed mycelium and no large fruiting body. The mold is ubiquitous in our lives, and is favored in warm and humid environments, and can be propagated in large quantities once in a suitable environment. The bred mould can generate a large amount of spores which are scattered in the air, so that the ambient air is full of mould flavor, people generate anaphylactic reaction and invade human bodies, and the kicking-off, urticaria, allergic rhinitis, mildew-removing disease and the like can be caused, meanwhile, mould spots can be formed on attachments, and the performance and the attractiveness of the attachments are greatly damaged.
The mildew remover in the prior art is in a liquid state, a foam state and a jelly state, wherein in the spraying process of the liquid state, not only can mildew spores be scattered due to liquid column impact, but also the liquid state can not be well adhered to the surface of pollutants, the action time is greatly reduced, the foam state can cause the reduction of the amount of the mildew remover actually contacted with an action surface due to the fact that a large amount of gas is mixed to form foam, the mildew removing effect is influenced, and compared with the liquid state mildew remover and the foam state mildew remover, the jelly-like mildew remover has better adhesiveness, but most of the prior mildew removers are prepared from chemical substances, and the mildew remover is strong in irritation, poor in environmental protection performance and needs to be further improved in adhesive force.
Disclosure of Invention
Aiming at the problems, the invention aims to disclose environment-friendly mildew-removing jelly and a preparation method thereof, wherein the environment-friendly mildew-removing jelly has better adhesive property through the synergistic effect of the raw materials, can be better attached to the surface of an object to be acted in the using process, can kill mildew in time, and can achieve the long-acting mildew-removing effect by forming a film layer on the surface of the mildew and combining mildew-removing microcapsules in the interior of the film layer.
Specifically, the environment-friendly mildew-removing gel provided by the invention comprises the following raw materials in parts by weight: 80-100 parts of imazalil, 20-40 parts of glycerol, 10-30 parts of beeswax, 10-20 parts of sodium starch octenyl succinate, 10-20 parts of polycaprolactone and 30-40 parts of mould-removing microcapsules.
Further, the environment-friendly mildew-removing jelly comprises the following raw materials in parts by weight: 90 parts of imazalil, 25 parts of glycerol, 20 parts of beeswax, 18 parts of starch sodium octenyl succinate, 15 parts of polycaprolactone and 35 parts of mould-removing microcapsules.
Furthermore, the mould removing microcapsule takes black tea extract as a capsule core and modified cyclodextrin as a capsule shell, and mould removing particles are dispersed in the black tea extract.
Further, the mould removing particles are porous carbon particles loaded with zero-valent iron.
In addition, the application also discloses a preparation method of the environment-friendly mildew-removing jelly, which specifically comprises the following steps:
s1: adding octenyl succinic acid starch sodium into deionized water, heating to 65-80 deg.C in water bath, stirring continuously until octenyl succinic acid starch sodium is dissolved, adding polyvinyl alcohol, stirring, adding glycerol and Cera flava, stirring for 40-60min, cooling to room temperature, adding polycaprolactone and imazalil, and stirring to obtain medicinal liquid;
s2: heating the obtained liquid medicine to 65-70 deg.C in water bath, stirring for 5-10min, adding mould removing microcapsule, ultrasonic dispersing for 20-30min, standing for 2h, freezing at-10-0 deg.C for 2-5h, taking out, and standing at room temperature for 30-40min to obtain mould removing gel.
Further, the preparation method of the mould removing microcapsule comprises the following steps: ultrasonically dispersing mildew-removing particles in a black tea extracting solution to obtain a suspension, adding modified cyclodextrin into deionized water, ultrasonically dissolving to obtain a modified cyclodextrin solution with the mass concentration of 40-45%, continuously stirring, adding into the suspension, continuously stirring for 0.5h to obtain a mixed solution, placing the mixed solution in an ice water bath for cooling, stirring for 30-45min, filtering, and drying to obtain the mildew-removing microcapsule.
Furthermore, the volume ratio of the suspension to the modified cyclodextrin solution is 1 (3-4).
Further, the preparation method of the modified cyclodextrin comprises the following steps: stirring and dissolving modified cyclodextrin in hot water of 50-60 ℃, adding hydrogen peroxide for reflux treatment for 3-4h, filtering, washing with deionized water to be neutral, freeze-drying and grinding into powder, adding the powder into water, heating in water bath to 80-95 ℃, stirring and dissolving under the protection of nitrogen, adding polyethylene glycol monomethyl ether and triethylamine, stirring and reacting for 24-48h, centrifuging after the reaction is finished, respectively cleaning the solid with absolute ethyl alcohol and deionized water for 3 times, placing the solid in a dialysis bag for dialysis for 48h, and performing dialysis and vacuum drying to obtain the modified cyclodextrin.
Further, the preparation method of the mildew removing particle comprises the following steps: adding iron sulfate heptahydrate into deionized water, stirring for dissolving, adding absolute ethyl alcohol, stirring uniformly, adding nano porous carbon, stirring for 3-4h by magnetic force, standing for 24-48h, dropwise adding a sodium tetrahydroborate solution under a stirring state until a large amount of bubbles are not generated in a reaction liquid, stopping dropwise adding, continuously stirring until the reaction liquid does not generate bubbles, performing suction filtration, washing a filter cake with the deionized water and the absolute ethyl alcohol for three times respectively, and performing vacuum drying to obtain the mildew-removing particles.
The invention has the beneficial effects that:
1. the invention discloses environment-friendly mildew-removing jelly, which can kill generated mildew through imazalil, can prolong the mildew-removing action time and effect through mildew-removing microcapsules, can effectively improve the viscosity of liquid medicine through added octenyl succinic acid starch sodium, can enable the mildew-removing jelly to be better adhered to attachments, and can enable the liquid medicine to have good film-forming property and plasticity through the synergistic effect of added beeswax, glycerin and polycaprolactone, so that a film can be quickly formed on the surface of the attachments in the using process, the mildew-removing microcapsules can be prevented from falling off, and meanwhile, mildew spores can be wrapped in the mildew-removing jelly to prevent the mildew spores from being dispersed everywhere.
2. According to the mould removing microcapsule disclosed by the invention, the modified cyclodextrin is used as the capsule shell, and the polyethylene glycol monomethyl ether is grafted to the cyclodextrin, so that the cyclodextrin has a temperature-sensitive property, and finally the capsule shell of the capsule has the temperature-sensitive property.
Detailed Description
The present invention will be described in detail below with reference to specific examples:
example one
Preparation of mildew removing particles:
adding 12g of iron sulfate heptahydrate into 100ml of deionized water, stirring and dissolving, adding 5ml of absolute ethyl alcohol, stirring and uniformly mixing, adding 5.6g of nano porous carbon, magnetically stirring for 3h, standing for 48h, then dropwise adding a sodium tetrahydroborate solution with the mass concentration of 550g/L under the stirring state until a large amount of bubbles are not generated in the reaction solution, stopping dropwise adding, continuously stirring until the reaction solution does not generate bubbles, performing suction filtration, washing filter cakes with the deionized water and the absolute ethyl alcohol for three times respectively, and performing vacuum drying at the temperature of 50 ℃ to obtain the mildew-removing particles.
Preparation of modified cyclodextrins
Weighing 1g of modified cyclodextrin, stirring and dissolving in 300ml of hot water at 55 ℃, adding 50ml of hydrogen peroxide, performing reflux treatment for 3 hours, filtering, washing a filter cake with deionized water until a washing solution is neutral, performing freeze drying, grinding into powder, adding into 500ml of water, heating in a water bath to 95 ℃, stirring and dissolving under the protection of nitrogen, adding 5g of polyethylene glycol monomethyl ether and 0.05g of triethylamine, stirring and reacting for 24 hours, centrifuging after the reaction is finished, respectively cleaning the solid with anhydrous absolute ethyl alcohol and deionized water for 3 times, placing in a dialysis bag, dialyzing with deionized water for 48 hours, completing dialysis, and performing vacuum drying to obtain the modified cyclodextrin.
Preparation of mould-removing microcapsule
Taking mildew-removing particles, stirring and dispersing the mildew-removing particles in a black tea extracting solution to obtain 15wt% turbid liquid, adding modified cyclodextrin into deionized water, performing ultrasonic dissolution to obtain a 45% modified cyclodextrin solution, continuously stirring, adding the modified cyclodextrin solution into the turbid liquid according to the volume ratio of 3:1, continuously stirring for 0.5h to obtain a mixed solution, placing the mixed solution in an ice water bath for cooling, stirring for 45min, filtering, and performing freeze drying to obtain the mildew-removing microcapsule.
Preparation of mould-removing jelly
S1: adding 18 parts of sodium starch octenyl succinate in 40 parts of deionized water, heating to 80 ℃, continuously stirring until the sodium starch octenyl succinate is dissolved, adding 3 parts of polyvinyl alcohol, stirring uniformly, adding 25 parts of glycerol and 20 parts of beeswax, continuously stirring for 50min, cooling to room temperature, adding 15 parts of polycaprolactone and 90 parts of imazalil, and stirring uniformly to obtain a liquid medicine;
s2: heating the obtained liquid medicine to 70 ℃ in a water bath, stirring for 5-10min, adding 35 parts of mould removing microcapsules, dispersing for 25min under the condition of 35KHz ultrasonic waves, standing for 2h, freezing for 2h at-10-0 ℃, taking out, and standing for 35min at room temperature to obtain the mould removing gel.
Example two
Preparation of mildew removing particles:
adding 11g of iron sulfate heptahydrate into 100ml of deionized water, stirring and dissolving, adding 5ml of absolute ethyl alcohol, stirring and uniformly mixing, adding 4.8g of nano porous carbon, magnetically stirring for 4h, standing for 24h, then dropwise adding a sodium tetrahydroborate solution with the mass concentration of 550g/L in the stirring state until a large amount of bubbles are not generated in the reaction solution, stopping dropwise adding, continuously stirring until the reaction solution does not generate bubbles, performing suction filtration, washing filter cakes with the deionized water and the absolute ethyl alcohol for three times respectively, and performing vacuum drying at the temperature of 60 ℃ to obtain the mildew-removing particles
Preparation of modified cyclodextrins
Weighing 1.23g of cyclodextrin, stirring and dissolving in 350ml of 50 ℃ hot water, adding 60ml of hydrogen peroxide, refluxing for 3h, filtering, washing a filter cake with deionized water until a washing solution is neutral, grinding into powder after freeze drying, adding into 500ml of water, heating in water bath to 80 ℃, stirring and dissolving under the protection of nitrogen, adding 5.5g of polyethylene glycol monomethyl ether and 0.06g of triethylamine, stirring and reacting for 48h, centrifuging after the reaction is finished, respectively cleaning the solid with absolute ethyl alcohol and deionized water for 3 times, placing in a dialysis bag, dialyzing with deionized water for 48h, completing dialysis, and performing vacuum drying to obtain the modified cyclodextrin.
Preparation of mould-removing granule microcapsule
Taking mildew-removing particles, stirring and dispersing the mildew-removing particles in a black tea extracting solution to obtain 15wt% suspension, adding modified cyclodextrin into deionized water, performing ultrasonic dissolution to obtain a modified cyclodextrin solution with the mass concentration of 45%, continuously stirring, adding the modified cyclodextrin solution into the suspension according to the volume ratio of 4:1, continuously stirring for 0.5h to obtain a mixed solution, placing the mixed solution in an ice water bath for cooling, stirring for 40min, filtering, and performing freeze drying to obtain the mildew-removing microcapsule.
Preparation of mould-removing jelly
S1: adding 10 parts of sodium starch octenylsuccinate into 40 parts of deionized water, heating the mixture to 65 ℃ in a water bath, continuously stirring the mixture until the sodium starch octenylsuccinate is dissolved, adding 4 parts of polyvinyl alcohol, stirring the mixture uniformly, adding 20 parts of glycerol and 10 parts of beeswax, continuously stirring the mixture for 40min, cooling the mixture to room temperature, adding 20 parts of polycaprolactone and 80 parts of imazalil, and stirring the mixture uniformly to obtain a liquid medicine;
s2: heating the obtained liquid medicine to 65 ℃ in water bath, stirring for 5-10min, adding 30 parts of mould removing microcapsule, dispersing for 20min under the ultrasonic condition with the frequency of 30KHz, standing for 2h, freezing for 3h at-10-0 ℃, taking out, and standing for 30min at room temperature to obtain the mould removing gel.
EXAMPLE III
Preparation of mildew removing particles:
adding 15g of iron sulfate heptahydrate into 100ml of deionized water, stirring and dissolving, adding 5ml of absolute ethyl alcohol, stirring and uniformly mixing, adding 7g of nano porous carbon, magnetically stirring for 4h, standing for 40h, then dropwise adding a sodium tetrahydroborate solution with the mass concentration of 550g/L in the stirring state until a large amount of bubbles are not generated in the reaction solution, stopping dropwise adding, continuously stirring until the reaction solution does not generate bubbles, performing suction filtration, washing filter cakes with the deionized water and the absolute ethyl alcohol for three times respectively, and performing vacuum drying at the temperature of 55 ℃ to obtain the mildew-removing particles
Preparation of modified cyclodextrins
Weighing 0.94g of cyclodextrin, stirring and dissolving in 300ml of 60 ℃ hot water, adding 45ml of hydrogen peroxide, carrying out reflux treatment for 4 hours, filtering, washing a filter cake with deionized water until a washing solution is neutral, carrying out freeze drying, grinding into powder, adding into 500ml of water, heating in a water bath to 85 ℃, stirring and dissolving under the protection of nitrogen, adding 4.8g of polyethylene glycol monomethyl ether and 0.04g of triethylamine, stirring and reacting for 36 hours, centrifuging after the reaction is finished, respectively cleaning the solid with absolute ethyl alcohol and deionized water for 3 times, placing in a dialysis bag, dialyzing with deionized water for 48 hours, finishing the dialysis, and carrying out vacuum drying to obtain the modified cyclodextrin.
Preparation of mould-removing granule microcapsule
Taking mildew-removing particles, stirring and dispersing the mildew-removing particles in a black tea extracting solution to obtain 15wt% suspension, adding modified cyclodextrin into deionized water, performing ultrasonic dissolution to obtain a modified cyclodextrin solution with the mass concentration of 45%, continuously stirring, adding the modified cyclodextrin solution into the suspension according to the volume ratio of 4:1, continuously stirring for 0.5h to obtain a mixed solution, placing the mixed solution in an ice water bath for cooling, stirring for 30min, filtering, and performing freeze drying to obtain the mildew-removing microcapsule.
Preparation of mould-removing jelly
S1: adding 20 parts of sodium starch octenylsuccinate into 40 parts of deionized water, heating to 70 ℃ in a water bath, continuously stirring until the sodium starch octenylsuccinate is dissolved, adding 5 parts of polyvinyl alcohol, stirring uniformly, adding 40 parts of glycerol and 30 parts of beeswax, continuously stirring for 60min, cooling to room temperature, adding 10 parts of polycaprolactone and 100 parts of imazalil, and stirring uniformly to obtain a liquid medicine;
s2: heating the obtained liquid medicine to 70 ℃ in a water bath, stirring for 5-10min, adding 40 parts of mould removing microcapsules, dispersing for 30min under the condition of 35KHz ultrasonic waves, standing for 2h, freezing for 5h at-10-0 ℃, taking out, and standing for 40min at room temperature to obtain the mould removing gel.
Comparative example 1
Compared with the first example, the difference of the comparison example is that the mildew-removing jelly of the comparison example does not add mildew-removing microcapsules in the raw materials.
Comparative example No. two
Compared with the first example, the difference of the comparison example is that the mildew-removing jelly of the comparison example does not add mildew-removing particles in the preparation process of the mildew-removing microcapsule.
The mildew-removing jelly prepared in the first example, the first comparative example and the second comparative example is used for a mildew-removing experiment, and meanwhile, the existing mildew-removing jelly in the market is purchased as a comparison, and the specific operation is as follows:
taking four vertical white walls with the same size and mass, sterilizing the white walls, inoculating moulds, controlling the air humidity to be more than 75%, culturing the white walls for one week at the temperature of 25-30 ℃, detecting the initial amount of the moulds on each white wall, then respectively and uniformly smearing 3mL of the mould removing gel prepared in the first embodiment, the first comparative example and the second comparative example and purchased mould removing gel, continuously culturing the white walls, detecting the bacterial content on the white walls once every 2 days until the mould spots on the surfaces of the white walls are dissolved, wherein the detection results are shown in Table 1:
TABLE 1
Figure BDA0003863755200000071
Figure BDA0003863755200000081
The data in the table show that the mildew removing gel prepared by the invention has good adhesion to an acting substance and can form a film quickly, mildew spots can be effectively removed under the action of the mildew removing microcapsule and the mildew removing particle, and meanwhile, a long-acting mildew removing effect is achieved.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.

Claims (9)

1. The environment-friendly mildew-removing gel is characterized by comprising the following raw materials in parts by weight: 80-100 parts of imazalil, 20-40 parts of glycerol, 10-30 parts of beeswax, 10-20 parts of sodium starch octenyl succinate, 10-20 parts of polycaprolactone and 30-40 parts of mould-removing microcapsules.
2. The environment-friendly type mildew-removing jelly according to claim 1, which is characterized by comprising the following raw materials in parts by weight: 90 parts of imazalil, 25 parts of glycerol, 20 parts of beeswax, 18 parts of starch sodium octenyl succinate, 15 parts of polycaprolactone and 35 parts of mould-removing microcapsules.
3. The environment-friendly type mildew-removing jelly as claimed in claim 2, wherein the mildew-removing microcapsule takes black tea extract as a capsule core and modified cyclodextrin as a capsule shell, and mildew-removing particles are dispersed in the black tea extract.
4. The environment-friendly mildew-removing jelly as claimed in claim 3, wherein the mildew-removing particles are porous carbon particles loaded with zero-valent iron.
5. The preparation method of the environment-friendly type mildew-removing jelly as claimed in any one of claims 1-4, wherein the preparation method specifically comprises the following steps:
s1: adding octenyl succinic acid starch sodium into deionized water, heating to 65-80 deg.C in water bath, stirring continuously until octenyl succinic acid starch sodium is dissolved, adding polyvinyl alcohol, stirring, adding glycerol and Cera flava, stirring for 40-60min, cooling to room temperature, adding polycaprolactone and imazalil, and stirring to obtain medicinal liquid;
s2: heating the obtained liquid medicine to 65-70 deg.C in water bath, stirring for 5-10min, adding mould removing microcapsule, ultrasonic dispersing for 20-30min, standing for 2h, freezing at-10-0 deg.C for 2-5h, taking out, and standing at room temperature for 30-40min to obtain mould removing gel.
6. The preparation method of the environment-friendly mildew-removing jelly as claimed in claim 5, wherein the preparation method of the mildew-removing microcapsule is as follows: ultrasonically dispersing mildew-removing particles in a black tea extracting solution to obtain a suspension, adding modified cyclodextrin into deionized water, ultrasonically dissolving to obtain a modified cyclodextrin solution with the mass concentration of 40-45%, continuously stirring, adding into the suspension, continuously stirring for 0.5h to obtain a mixed solution, placing the mixed solution in an ice water bath for cooling, stirring for 30-45min, filtering, and drying to obtain the mildew-removing microcapsule.
7. The method for preparing environment-friendly mildew-removing jelly as claimed in claim 6, wherein the volume ratio of the suspension to the modified cyclodextrin solution is 1 (3-4).
8. The preparation method of the environment-friendly type mildew-removing gel according to claim 7, wherein the preparation method of the modified cyclodextrin comprises the following steps: stirring and dissolving modified cyclodextrin in hot water of 50-60 ℃, adding hydrogen peroxide for reflux treatment for 3-4h, filtering, washing with deionized water to be neutral, freeze-drying and grinding into powder, adding the powder into water, heating in water bath to 80-95 ℃, stirring and dissolving under the protection of nitrogen, adding polyethylene glycol monomethyl ether and triethylamine, stirring and reacting for 24-48h, centrifuging after the reaction is finished, respectively cleaning the solid with absolute ethyl alcohol and deionized water for 3 times, placing the solid in a dialysis bag for dialysis for 48h, and performing dialysis and vacuum drying to obtain the modified cyclodextrin.
9. The preparation method of the environment-friendly mildew-removing jelly as claimed in claim 8, wherein the preparation method of the mildew-removing granule is as follows: adding iron sulfate heptahydrate into deionized water, stirring for dissolving, adding absolute ethyl alcohol, stirring uniformly, adding nano porous carbon, stirring for 3-4h by magnetic force, standing for 24-48h, dropwise adding a sodium tetrahydroborate solution under a stirring state until a large amount of bubbles are not generated in a reaction liquid, stopping dropwise adding, continuously stirring until the reaction liquid does not generate bubbles, performing suction filtration, washing a filter cake with the deionized water and the absolute ethyl alcohol for three times respectively, and performing vacuum drying to obtain the mildew-removing particles.
CN202211172363.4A 2022-09-26 2022-09-26 Environment-friendly mildew-removing gel and preparation method thereof Pending CN115644184A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111165476A (en) * 2020-01-03 2020-05-19 中国人民解放军陆军军医大学第二附属医院 Mildew-proof mildew-removing agent for ceiling and preparation method thereof
CN111642788A (en) * 2020-05-11 2020-09-11 重庆中烟工业有限责任公司 Biological preparation capsule containing bacillus cereus

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111165476A (en) * 2020-01-03 2020-05-19 中国人民解放军陆军军医大学第二附属医院 Mildew-proof mildew-removing agent for ceiling and preparation method thereof
CN111642788A (en) * 2020-05-11 2020-09-11 重庆中烟工业有限责任公司 Biological preparation capsule containing bacillus cereus

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