Efficient bamboo and wood mildew preventive and preparation method thereof

Abstract

The invention discloses an efficient bamboo wood mildew inhibitor and a preparation method thereof, and relates to the field of mildew inhibitors, the efficient bamboo wood mildew inhibitor comprises the following raw materials by weight: 0.1-5 parts of mildew-proof composite particles, 80-90 parts of a solvent, 0.2-3 parts of a dispersion liquid, and 5-10 parts of a film-forming agent; the preparation method of the mildewproof composite particles comprises the following steps: firstly preparing rod-point particles with amino groups, and then adding a copper ion solution, thereby obtaining the mildewproof composite particles, the mildew-proof composite particles are added into the mildew-proof agent, rod-point particles with amino groups are complexed with copper ions in the mildew-proof composite particles to form a substance with stable mildew-proof performance, and raspberry structure particles are attached to the surface of graphene oxide to obtain a specific rod-point structure, so that the mildew-proof agent has good hydrophobicity; in the use process of the mildew preventive, the contact between moisture and bamboos is reduced, and the possibility of mildew is greatly reduced.

Description

Technical Field

[0001] The present invention relates to the field of mildew inhibitors, and in particular to a high-efficiency mildew inhibitor for bamboo and wood and a preparation method thereof. Background Art

[0002] Mold inhibitors are a type of polymer material that can inhibit the growth of mold and kill mold. Generally, there are natural mold inhibitors and synthetic mold inhibitors.

[0003] China boasts abundant bamboo resources, and its production and consumption of bamboo products rank among the highest in the world. However, during the bamboo processing and production process, mildew often occurs. This not only affects the aesthetics of bamboo products and creates an unpleasant odor, but also, as wood is a key component of home furnishings, can lead to mildew during use due to poor craftsmanship. This can also degrade the quality of bamboo products, reducing their compressive and tensile strength. Mold inhibitors can effectively prevent mildew, so developing a suitable mold inhibitor for bamboo and wood is of great importance.

[0004] However, most current mold inhibitors are organic. Due to their complex functional groups, they are prone to chemical reactions when mixed with other mold inhibitors or organic compounds, even producing precipitation, which compromises their effectiveness. Existing technologies have yet to address the issues of non-stratification, non-precipitation, and poor mold prevention effectiveness of mold inhibitors. Summary of the Invention

[0005] The purpose of the present invention is to solve at least one of the technical problems existing in the prior art and to provide a high-efficiency bamboo and wood mildew inhibitor and a preparation method thereof.

[0006] The technical solutions of the present invention are as follows:

[0007] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0008] 0.1-5 parts of anti-mildew composite particles, 80-90 parts of solvent, 0.2-3 parts of dispersion liquid, and 5-10 parts of film-forming agent;

[0009] The preparation method of the mildew-proof composite particles is as follows:

[0010] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0011] The preparation method of the rod-point particles having amino groups:

[0012] The surface of graphene oxide is modified with dopamine hydrochloride, and then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 50-70° C. for 10-30 hours, and then heptadecafluorodecyltriethoxysilane is added dropwise, and the reaction is continued for 4-8 hours. After the reaction, the product is rinsed and dried.

[0013] Preferably, the preparation method of the raspberry-like nanoparticles is as follows:

[0014] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 10-20 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, sodium hydroxide solution is added continuously, oxygen is introduced and stirred, and polymer microspheres are added at the same time to obtain the product.

[0015] Preferably, the dispersion is prepared as follows:

[0016] Zinc acetate dihydrate and nano-titanium dioxide are added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 100-200°C for 3-4 hours.

[0017] Preferably, the mass ratio of zinc acetate dihydrate, nano-titanium dioxide and diethylene glycol is 3:5-8:10.

[0018] Preferably, the copper ion solution is 2-5 mg / L.

[0019] Preferably, the film-forming agent is polyvinyl alcohol.

[0020] Preferably, the mass addition ratio of the copper ion solution to the amino group-containing rod-point particles is 3-5:6.

[0021] Preferably, the mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3-5:0.5-1:0.5-1:0.5-1.

[0022] The invention also discloses a preparation method of a high-efficiency bamboo and wood mildew inhibitor, which comprises mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 10-30 minutes at a stirring speed of 100-300 rpm and a stirring temperature of 40-60° C., and sealing to obtain the agent.

[0023] The beneficial effects of the present invention are:

[0024] The present invention incorporates mildew-resistant composite particles into a mildew-resistant agent. The mildew-resistant composite particles utilize amino-containing rod-point particles to complex with copper ions, forming a stable mildew-resistant material. Furthermore, raspberry-structured particles are attached to the surface of graphene oxide to create a specific rod-point structure. This structure imparts excellent hydrophobicity, preventing moisture from contacting bamboo and wood during use, significantly reducing the likelihood of mildew. Furthermore, the added dispersion contains a composite of nano-zinc oxide and titanium dioxide, which can bind to phenolic hydroxyl groups on bamboo and wood to form stable chemical bonds, penetrate deep tissue layers, and reduce leaching. Simultaneously, the composite, in combination with a film-forming agent, can form a non-displaceable film on the bamboo and wood surface, significantly enhancing the mildew-resistant agent's adhesion. Furthermore, the titanium dioxide exhibits photosensitivity and antioxidant properties. DETAILED DESCRIPTION

[0025] The following embodiments of the present invention are described in detail. The embodiments described below are exemplary and are only used to explain the present invention, and are not to be construed as limiting the present invention. Where specific techniques or conditions are not specified in the embodiments, the techniques or conditions described in the literature in this field or the product specifications are used. Where the manufacturer of the reagents or instruments is not specified, all are conventional products that can be obtained commercially.

[0026] The solvent is specifically: a mixture of ethanol and water in a ratio of 7:3 by volume.

[0027] Example 1

[0028] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0029] 3 parts of anti-mildew composite particles, 85 parts of solvent, 3 parts of dispersion liquid, and 8 parts of film-forming agent;

[0030] The preparation method of the mildew-proof composite particles is as follows:

[0031] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0032] The preparation method of the rod-point particles having amino groups:

[0033] The surface of graphene oxide was modified with 2 g / L dopamine hydrochloride by stirring for 24 hours, then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 60° C. for 24 hours, and then heptadecafluorodecyltriethoxysilane was added dropwise and the reaction was continued for 5 hours. After the reaction, the surface was rinsed and dried to obtain the product.

[0034] The preparation method of the raspberry-like nanoparticles is as follows:

[0035] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 18 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, and 2 mol / L sodium hydroxide solution is added. Oxygen is introduced and stirred, and polymer microspheres (3 μm polystyrene microspheres) are added at the same time to obtain the product.

[0036] The dispersion was prepared as follows:

[0037] Zinc acetate dihydrate and nano-titanium dioxide were added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 180°C for 3h.

[0038] The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:8:10.

[0039] The copper ion solution is a 2 mg / L copper chloride solution.

[0040] The film-forming agent is polyvinyl alcohol.

[0041] The mass addition ratio of the copper ion solution to the rod-point particles having amino groups is 1:2.

[0042] The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.5:0.7:1.

[0043] A preparation method of a high-efficiency bamboo and wood mildew inhibitor comprises the following steps: mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 20 minutes at a stirring speed of 200 rpm and a stirring temperature of 50° C., and sealing to obtain the agent.

[0044] Example 2

[0045] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0046] 3 parts of anti-mildew composite particles, 85 parts of solvent, 3 parts of dispersion liquid, and 8 parts of film-forming agent;

[0047] The preparation method of the mildew-proof composite particles is as follows:

[0048] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0049] The preparation method of the rod-point particles having amino groups:

[0050] The surface of graphene oxide was modified with 2 g / L dopamine hydrochloride by stirring for 24 hours, then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 60° C. for 24 hours, and then heptadecafluorodecyltriethoxysilane was added dropwise and the reaction was continued for 5 hours. After the reaction, the surface was rinsed and dried to obtain the product.

[0051] The preparation method of the raspberry-like nanoparticles is as follows:

[0052] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 18 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, and 2 mol / L sodium hydroxide solution is added. Oxygen is introduced and stirred, and polymer microspheres (3 μm polystyrene microspheres) are added at the same time to obtain the product.

[0053] The dispersion was prepared as follows:

[0054] Zinc acetate dihydrate and nano-titanium dioxide were added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 180°C for 3h.

[0055] The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:8:10.

[0056] The copper ion solution is a 3 mg / L copper chloride solution.

[0057] The film-forming agent is polyvinyl alcohol.

[0058] The mass addition ratio of the copper ion solution to the rod-point particles having amino groups is 1:2.

[0059] The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.5:0.7:1.

[0060] A preparation method of a high-efficiency bamboo and wood mildew inhibitor comprises the following steps: mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 20 minutes at a stirring speed of 200 rpm and a stirring temperature of 50° C., and sealing to obtain the agent.

[0061] Example 3

[0062] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0063] 3 parts of anti-mildew composite particles, 85 parts of solvent, 3 parts of dispersion liquid, and 8 parts of film-forming agent;

[0064] The preparation method of the mildew-proof composite particles is as follows:

[0065] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0066] The preparation method of the rod-point particles having amino groups:

[0067] The surface of graphene oxide was modified with 2 g / L dopamine hydrochloride by stirring for 24 hours, then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 60° C. for 24 hours, and then heptadecafluorodecyltriethoxysilane was added dropwise and the reaction was continued for 5 hours. After the reaction, the surface was rinsed and dried to obtain the product.

[0068] The preparation method of the raspberry-like nanoparticles is as follows:

[0069] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 18 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, and 2 mol / L sodium hydroxide solution is added. Oxygen is introduced and stirred, and polymer microspheres (3 μm polystyrene microspheres) are added at the same time to obtain the product.

[0070] The dispersion was prepared as follows:

[0071] Zinc acetate dihydrate and nano-titanium dioxide were added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 180°C for 3h.

[0072] The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:8:10.

[0073] The copper ion solution is a 5 mg / L copper chloride solution.

[0074] The film-forming agent is polyvinyl alcohol.

[0075] The mass addition ratio of the copper ion solution to the rod-point particles having amino groups is 1:2.

[0076] The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.5:0.7:1.

[0077] A preparation method of a high-efficiency bamboo and wood mildew inhibitor comprises the following steps: mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 20 minutes at a stirring speed of 200 rpm and a stirring temperature of 50° C., and sealing to obtain the agent.

[0078] Example 4

[0079] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0080] 3 parts of anti-mildew composite particles, 85 parts of solvent, 3 parts of dispersion liquid, and 8 parts of film-forming agent;

[0081] The preparation method of the mildew-proof composite particles is as follows:

[0082] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0083] The preparation method of the rod-point particles having amino groups:

[0084] The surface of graphene oxide was modified with 2 g / L dopamine hydrochloride by stirring for 24 hours, then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 60° C. for 24 hours, and then heptadecafluorodecyltriethoxysilane was added dropwise and the reaction was continued for 5 hours. After the reaction, the surface was rinsed and dried to obtain the product.

[0085] The preparation method of the raspberry-like nanoparticles is as follows:

[0086] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 18 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, and 2 mol / L sodium hydroxide solution is added. Oxygen is introduced and stirred, and polymer microspheres (3 μm polystyrene microspheres) are added at the same time to obtain the product.

[0087] The dispersion was prepared as follows:

[0088] Zinc acetate dihydrate and nano-titanium dioxide were added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 180°C for 3h.

[0089] The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:8:10.

[0090] The copper ion solution is a 3 mg / L copper chloride solution.

[0091] The film-forming agent is polyvinyl alcohol.

[0092] The mass addition ratio of the copper ion solution to the amino group-containing rod-point particles is 2:3.

[0093] The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.5:0.7:1.

[0094] A preparation method of a high-efficiency bamboo and wood mildew inhibitor comprises the following steps: mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 20 minutes at a stirring speed of 200 rpm and a stirring temperature of 50° C., and sealing to obtain the agent.

[0095] Example 5

[0096] A highly effective bamboo and wood mildew inhibitor comprising the following raw materials in parts by weight:

[0097] 3 parts of anti-mildew composite particles, 85 parts of solvent, 3 parts of dispersion liquid, and 8 parts of film-forming agent;

[0098] The preparation method of the mildew-proof composite particles is as follows:

[0099] First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain;

[0100] The preparation method of the rod-point particles having amino groups:

[0101] The surface of graphene oxide was modified with 2 g / L dopamine hydrochloride by stirring for 24 hours, then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 60° C. for 24 hours, and then heptadecafluorodecyltriethoxysilane was added dropwise and the reaction was continued for 5 hours. After the reaction, the surface was rinsed and dried to obtain the product.

[0102] The preparation method of the raspberry-like nanoparticles is as follows:

[0103] After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 18 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, and 2 mol / L sodium hydroxide solution is added. Oxygen is introduced and stirred, and polymer microspheres (3 μm polystyrene microspheres) are added at the same time to obtain the product.

[0104] The dispersion was prepared as follows:

[0105] Zinc acetate dihydrate and nano-titanium dioxide were added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 180°C for 3h.

[0106] The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:8:10.

[0107] The copper ion solution is a 3 mg / L copper chloride solution.

[0108] The film-forming agent is polyvinyl alcohol.

[0109] The mass addition ratio of the copper ion solution to the amino group-containing rod-point particles is 5:6.

[0110] The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.5:0.7:1.

[0111] A preparation method of a high-efficiency bamboo and wood mildew inhibitor comprises the following steps: mixing mildew-proof composite particles, a solvent and a dispersion liquid, stirring for 20 minutes at a stirring speed of 200 rpm and a stirring temperature of 50° C., and sealing to obtain the agent.

[0112] Example 6

[0113] Different from Example 2, the mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:0.8:0.9:1.

[0114] Example 7

[0115] Different from Example 2, the mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3:1:0.9:08.

[0116] Comparative Example 1

[0117] The difference from Example 2 is that the mildew-proof composite particles are a copper chloride solution.

[0118] Comparative Example 2

[0119] The difference from Example 2 is that the preparation method of the rod-point particles having amino groups is:

[0120] The graphene oxide surface was modified with 2 g / L dopamine hydrochloride by stirring for 24 h.

[0121] Comparative Example 3

[0122] The difference from Example 2 is that the preparation method of the rod-point particles having amino groups is:

[0123] The graphene oxide surface was modified with 2 g / L dopamine hydrochloride and stirred for 24 h, then immersed in a mixed solution of ammonia water and anhydrous ethanol, tetraethyl orthosilicate was added dropwise for reaction for 18 h, 3-glycidoxypropyltrimethoxysilane was added dropwise, and 2 mol / L sodium hydroxide solution was continued to be added.

[0124] Comparative Example 4

[0125] Different from Example 2, no dispersion liquid was added.

[0126] The above examples and comparative examples were subjected to performance tests, and the test results are shown in Table 1.

[0127] Delamination test: Place the sample under light and let it stand for 24 hours. Observe with the naked eye and there will be no reaction sediment or insoluble accumulation at the bottom of the liquid, that is, the anti-mildew liquid does not show delamination.

[0128] Mildew resistance testing: Using GB / T 1741-2020, "Determination of Mildew Resistance of Paint Films," the test was conducted by adding 20% by weight of the sample to the paint and stirring thoroughly. The mixed paint was then applied to a 5x5cm glass plate. A blank control group was used, with five samples per group. Mold spores were inoculated on the sample surface and then incubated at 28°C and 90% humidity for 28 days. Mold growth was observed and graded accordingly.

[0129] Mildew resistance level 0: no growth, mildew growing area 0%;

[0130] Mildew resistance level 1: trace growth, mildew area <10%;

[0131] Mildew resistance level 2: small amount of growth, 10% ≤ mildew growth area < 30%;

[0132] Mildew resistance level 3: moderate growth, 30% ≤ mildew area < 60%;

[0133] Mildew resistance level 4: Severe growth, mildew area ≥ 60%.

[0134] Table 1 Performance test results of the embodiments and comparative examples

[0135]

[0136]

[0137] Table 1 shows that the performance of the examples is superior to that of the comparative examples. This is likely due to the addition of anti-mildew composite particles to the anti-mildew agent, the use of amino-containing rod-point particles in the anti-mildew composite particles to complex with copper ions, forming a stable anti-mildew material. Furthermore, the use of raspberry-structured particles attached to the surface of graphene oxide creates a specific rod-point structure, which imparts excellent hydrophobicity. This prevents the anti-mildew agent from contacting bamboo and wood with water during use, significantly reducing the risk of mildew and improving the stability of the anti-mildew agent. Furthermore, the added dispersion contains a composite of nano-zinc oxide and titanium dioxide, which can bind to the phenolic hydroxyl groups on the bamboo and wood to form a stable chemical bond, penetrate deep tissue, and reduce its leaching rate. Furthermore, the combination with the film-forming agent can form a non-displaceable film on the bamboo and wood surface, significantly improving the adhesion of the anti-mildew agent. Furthermore, titanium dioxide has photosensitivity and antioxidant properties.

[0138] The above-described embodiments merely represent preferred implementations of the present invention. While the descriptions thereof are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make various other corresponding changes and modifications based on the technical solutions and concepts described above, and all such changes and modifications should fall within the scope of protection of the claims of the present invention.

Claims

1. A high-efficiency bamboo and wood mildew inhibitor, characterized in that: The composition comprises the following raw materials in parts by weight: 0.1-5 parts of anti-mildew composite particles, 80-90 parts of solvent, 0.2-3 parts of dispersion liquid, and 5-10 parts of film-forming agent; The preparation method of the mildew-proof composite particles is as follows: First, rod-point particles with amino groups are prepared, and then copper ion solution is added to obtain; The preparation method of the rod-point particles having amino groups: The surface of graphene oxide is modified with dopamine hydrochloride, and then immersed in an ethanol dispersion of raspberry-like nanoparticles, reacted at 50-70° C. for 10-30 hours, and then heptadecafluorodecyltriethoxysilane is added dropwise, and the reaction is continued for 4-8 hours. After the reaction, the product is rinsed and dried.

2. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The preparation method of the raspberry-like nanoparticles is as follows: After ammonia water and anhydrous ethanol are evenly mixed, tetraethyl orthosilicate is added dropwise to react for 10-20 hours, 3-glycidyloxypropyltrimethoxysilane is added dropwise, sodium hydroxide solution is added continuously, oxygen is introduced and stirred, and polymer microspheres are added at the same time to obtain the product.

3. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The dispersion was prepared as follows: Zinc acetate dihydrate and nano-titanium dioxide are added to diethylene glycol, dissolved by ultrasonication, and then subjected to hydrothermal reaction at 100-200°C for 3-4 hours.

4. A high-efficiency bamboo and wood mildew inhibitor according to claim 3, characterized in that: The mass ratio of the zinc acetate dihydrate, nano titanium dioxide and diethylene glycol is 3:5-8:

10.

5. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The copper ion solution has an concentration of 2-5 mg / L.

6. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The film-forming agent is polyvinyl alcohol.

7. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The mass addition ratio of the copper ion solution to the amino group-containing rod-point particles is 3-5:

6.

8. A high-efficiency bamboo and wood mildew inhibitor according to claim 1, characterized in that: The mass ratio of the graphene oxide, dopamine hydrochloride, raspberry-like nanoparticles and heptadecafluorodecyltriethoxysilane is 3-5:0.5-1:0.5-1:0.5-1.

9. A method for preparing a high-efficiency bamboo and wood mildew inhibitor, characterized in that: The anti-mildew composite particles, solvent and dispersion are mixed, stirred for 10-30 minutes at a stirring speed of 100-300 rpm and a stirring temperature of 40-60° C., and sealed to obtain the product.

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