CN114736416B - Washable sun-proof emulsion and preparation method thereof - Google Patents
Washable sun-proof emulsion and preparation method thereof Download PDFInfo
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Abstract
The application relates to washable sun-proof emulsion, which comprises the following raw materials: latex glue, a compound vulcanizing agent, oleic acid and linseed oil; the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent and water. Also relates to a preparation method of the washable sun-proof emulsion, which comprises the preparation of the composite vulcanizing agent and the preparation of the finished product. According to the application, a polymer network is formed by polymerizing 2-ethylhexyl acrylate and 2-acetamido-3-dimethylaminomethyl acrylate, so that a concentrated continuous phase which is easy to be corroded by ultraviolet rays is reduced, and the anti-aging property and weather resistance are obtained; the product and 2-ethylhexyl acrylate are further synergistic; the 2-hydroxy-4-methoxyl benzophenone absorbs ultraviolet rays, and the latex product can be better sterilized by long-time irradiation of sunlight after being cleaned, and the service life is longer.
Description
Technical Field
The application relates to the technical field of latex, in particular to washable sun-proof latex and a preparation method thereof.
Background
With the development of economy and the improvement of the living standard of people, the latex products are widely produced in the living production of people, the existing latex products are mostly made of pure natural latex, and the natural latex products comprise latex pillows, latex mattresses, latex back cushions and the like, and have the advantages of mite prevention, bacteria prevention, good air permeability and hygroscopicity.
In view of the above-mentioned related art, the inventors consider that the existing latex products made of latex have poor aging resistance, which results in that the existing latex products cannot achieve the sterilization purpose by long-time irradiation of sunlight after cleaning, and the service lives thereof are correspondingly short, so that improvement is still needed.
Disclosure of Invention
In order to improve the ageing resistance of the latex and prolong the service life, the application provides washable sun-proof latex and a preparation method thereof.
In a first aspect, the washable sun-proof emulsion provided by the application adopts the following technical scheme:
the washable sun-proof emulsion comprises the following raw materials in parts by weight:
120-130 parts of latex glue;
10-15 parts of a composite vulcanizing agent;
4-6 parts of oleic acid;
1-2 parts of linseed oil;
the composite vulcanizing agent comprises the following components in parts by weight:
50-60 parts of sulfur;
10-12 parts of 2-ethylhexyl acrylate;
5-6 parts of 2-acetylamino-3-dimethylaminomethyl acrylate;
1-2 parts of an initiator;
10-15 parts of 2-hydroxy-4-methoxybenzophenone;
6-9 parts of dispersing agent;
36-45 parts of an accelerator;
0.5-0.6 part of ammonia water;
0.5-0.7 part of detergent;
120-130 parts of water.
By adopting the technical scheme, under the action of an initiator, 2-acetylamino-3-dimethylaminomethyl acrylate is added into 2-ethylhexyl acrylate and emulsion polymerization is carried out under the action of the initiator, so that 2-acetylamino-3-dimethylaminomethyl acrylate molecules are uniformly distributed in the 2-ethylhexyl acrylate to form a polymer network, thereby reducing concentrated continuous phases in the polymerization emulsion, which are easy to be corroded by ultraviolet rays, and enabling the polymerization emulsion to have good ageing resistance and weather resistance; the polymerization emulsion and the 2-ethylhexyl acrylate can be further polymerized, the synergistic effect is achieved, the polymer network density is higher, the existence of a continuous phase is further reduced, the component state of the obtained composite vulcanizing agent is more stable, and the 2-hydroxy-4-methoxybenzophenone further absorbs ultraviolet rays, so that the emulsion has more excellent ageing resistance; the dispersing agent has the functions of emulsification, dispersion and stabilization; therefore, the ageing resistance is improved, the latex product can be better sterilized by long-time irradiation of sunlight after being cleaned, and the service life is longer.
Preferably, the compound vulcanizing agent further comprises 1-2 parts of 1, 2-propylene diamine in parts by weight.
By adopting the technical scheme, the 1, 2-propylene diamine is used as the cross-linking agent, and the 2-acetylamino-3-dimethylaminomethyl acrylate can undergo intramolecular self-crosslinking polymerization reaction, so that a denser self-crosslinking network structure is formed, on one hand, the acrylic acid-2-ethylhexyl ester and a self-crosslinking product molecular chain can be crosslinked in a chemical bond mode, so that an interpenetrating network with a more stable structure is formed, and on the other hand, a crosslinked and polymerized structure can be formed between the interpenetrating network and a polymerized emulsion formed by the acrylic acid-2-ethylhexyl ester and the 2-acetylamino-3-dimethylaminomethyl acrylate, so that the aim of effectively improving the ageing resistance is fulfilled.
Preferably, the compound vulcanizing agent further comprises 2-3 parts by weight of tert-butylcatechol, 1-3 parts by weight of 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole and 1-2 parts by weight of antioxidant 616.
By adopting the technical scheme, the phenolic hydroxyl has the capability of providing protons, and captures alkyl free radicals to form a stable conjugated free radical structure before the alkyl free radicals are combined with oxygen to form alkyl peroxidation free radicals, and the free radical oxidation is blocked in the free radical chain initiation stage; the antioxidant of different types is compounded to obtain better oxidation resistance, and further compounding of the polymerization emulsion, tert-butylcatechol, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole and antioxidant 616 can play a role in better synergistic interaction, has excellent barrier property to oxygen, absorbs ultraviolet rays, has efficient light stabilization effect and has high ageing resistance.
Preferably, the compound vulcanizing agent further comprises 4-5 parts by weight of 4-methoxybenzaldehyde-3-sodium sulfonate and 0.4-0.6 part by weight of catalyst.
By adopting the technical scheme, the 4-methoxybenzaldehyde-3-sodium sulfonate is further added, and the thermal stability can be improved by catalyzing the condensation reaction of tert-butylcatechol and the 4-methoxybenzaldehyde-3-sodium sulfonate, so that the steric hindrance of the obtained product is larger, the relative molecular mass is increased; in addition, the group in the 4-methoxybenzaldehyde-3-sodium sulfonate and 2-hydroxy-4-methoxybenzophenone can generate condensation reaction due to the existence of alkaline ammonia water in the mixing process, so that a better composite effect is generated, and the ageing resistance is effectively improved.
Preferably, the catalyst is triethylamine.
Preferably, the initiator is potassium persulfate.
Preferably, the dispersing agent comprises sodium methylene dinaphthyl sulfonate and polyoxyethylene stearate, and the weight ratio of the sodium methylene dinaphthyl sulfonate to the polyoxyethylene stearate is 1:2.
Preferably, the accelerator comprises an accelerator M, an accelerator ZDC and an accelerator DPG, and the accelerator M is prepared from the following components in parts by weight: promoter ZDC: accelerator dpg=4:4:1.
In a second aspect, the application provides a method for preparing washable sun-proof emulsion, which adopts the following technical scheme:
a preparation method of washable sun-proof emulsion comprises the following steps:
s1, preparing a composite vulcanizing agent; mixing and stirring 2-acetylamino-3-dimethylamino methyl acrylate, an initiator, a dispersing agent and 40-50 parts of water at normal temperature for 5-6 hours, blowing nitrogen for 2 hours, adding 7-8 parts of 2-ethylhexyl acrylate, stirring and reacting at 50-60 ℃ for 50-60 minutes, and dispersing at a rotating speed of 300-600r/min for 15-20 minutes; then adding the rest 2-ethylhexyl acrylate, and dispersing for 5-10min at the rotating speed of 300-600r/min to obtain an emulsion product; then adding sulfur, 2-hydroxy-4-methoxyl diphenyl ketone, an accelerator, ammonia water, detergent and the rest water, and continuously stirring for 4-5 hours;
s2, preparing a finished product; mixing the latex glue, the composite vulcanizing agent prepared in the step S1, oleic acid and linseed oil at the temperature of 30-32 ℃, stirring for 18-22 hours, and then foaming, injection molding and demolding to prepare the latex product.
Preferably, the step S1 further includes the following steps:
blending 1-2 parts of 1, 2-propylene diamine, 5-6 parts of 2-acetylamino-3-dimethylaminomethyl acrylate and 8-10 parts of water, and stirring at 70-80 ℃ for 1-1.5 hours to obtain a mixture A; then, continuously adding 1-2 parts of initiator, 6-9 parts of dispersing agent and 40-50 parts of water into the mixture A, mixing and stirring for 5-6 hours at normal temperature, and blowing nitrogen for 2 hours, then adding 7-8 parts of 2-ethylhexyl acrylate, stirring and reacting for 50-60 minutes at 50-60 ℃, and dispersing for 15-20 minutes at the rotating speed of 300-600 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 5-10min at the rotating speed of 300-600r/min to obtain an emulsion product;
2-3 parts of tert-butylcatechol, 4-5 parts of 4-methoxybenzaldehyde-3-sodium sulfonate and 0.4-0.6 part of catalyst are mixed and stirred at 50-60 ℃ for reaction for 50-60min to obtain a mixture B;
mixing the mixture B and the emulsion product and continuously stirring for 30-40min; then 50-60 parts of sulfur, 10-15 parts of 2-hydroxy-4-methoxybenzophenone, 1-3 parts of 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, 1-2 parts of antioxidant 616, 36-45 parts of accelerator, 0.5-0.6 part of ammonia water, 0.5-0.7 part of detergent and the balance of water are added, and stirring is continued for 4-5 hours.
In summary, the application has the following beneficial technical effects:
1. under the action of an initiator, adding 2-acetamido-3-dimethylamino methyl acrylate into 2-ethylhexyl acrylate, and performing emulsion polymerization under the action of the initiator to uniformly distribute 2-acetamido-3-dimethylamino methyl acrylate molecules into the 2-ethylhexyl acrylate to form a polymer network, so that concentrated continuous phases which are easily corroded by ultraviolet rays in the polymerization emulsion are reduced, and the polymerization emulsion has good ageing resistance and weather resistance; the polymerization emulsion and the 2-ethylhexyl acrylate can be further polymerized, the synergistic effect is achieved, the polymer network density is higher, the existence of a continuous phase is further reduced, the component state of the obtained composite vulcanizing agent is more stable, and the 2-hydroxy-4-methoxybenzophenone further absorbs ultraviolet rays, so that the emulsion has more excellent ageing resistance; the dispersing agent has the functions of emulsification, dispersion and stabilization; therefore, the ageing resistance is improved, the latex product can be better sterilized by long-time irradiation of sunlight after being cleaned, and the service life is longer;
2. 1, 2-propylene diamine is used as a cross-linking agent, and 2-acetylamino-3-dimethylamino methyl acrylate can undergo intramolecular self-crosslinking polymerization reaction, so that a denser self-crosslinking network structure is formed, on one hand, the acrylic acid-2-ethylhexyl ester and a self-crosslinking product molecular chain can be crosslinked in a chemical bond mode, so that an interpenetrating network with a more stable structure is formed, and on the other hand, a crosslinked and polymerized structure can be formed between the obtained interpenetrating network and a polymerized emulsion formed by acrylic acid-2-ethylhexyl ester and 2-acetylamino-3-dimethylamino methyl acrylate, so that the aim of effectively improving ageing resistance is achieved;
3. the phenolic hydroxyl group has the capability of providing protons, and captures alkyl free radicals to form a stable conjugated free radical structure before the alkyl free radicals are combined with oxygen to form alkyl peroxidation free radicals, and blocks free radical oxidation in a free radical chain initiation stage; the antioxidant of different types is compounded to obtain better oxidation resistance, and further compounding of the polymerization emulsion, tert-butylcatechol, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole and antioxidant 616 can play a role in better synergistic interaction, has excellent barrier property to oxygen, absorbs ultraviolet rays, has efficient light stabilization effect and has high ageing resistance;
4. further adding 4-methoxybenzaldehyde-3-sodium sulfonate, and catalyzing the condensation reaction of tert-butylcatechol and 4-methoxybenzaldehyde-3-sodium sulfonate to obtain a product with larger steric hindrance and increased relative molecular mass, so that the thermal stability can be improved; in addition, the group in the 4-methoxybenzaldehyde-3-sodium sulfonate and 2-hydroxy-4-methoxybenzophenone can generate condensation reaction due to the existence of alkaline ammonia water in the mixing process, so that a better composite effect is generated, and the ageing resistance is effectively improved.
Drawings
FIG. 1 is the visual test results of the reference sample of the present application and the test samples of examples 1-3; the reference sample and the test samples of examples 1-3 are in order from left to right;
FIG. 2 is the visual test results of the reference sample of the present application and the test samples of examples 4-6; the reference samples and the test samples of examples 4-6 are shown in the order from left to right.
Detailed Description
The present application will be described in further detail below.
In the application, the latex glue is produced by Wenzhou glue grain International trade company, with the goods number 20200302; oleic acid was produced by shandong sheng long chemical company, inc; linseed oil is produced by the company of the chemical company of Jianer, guangzhou; polyoxyethylene stearate is produced by Jiangsu Estragaceae chemical Co., ltd; t-butylcatechol is produced by Jin Jinle chemical company, inc.
The raw materials used in the following embodiments may be commercially available from ordinary sources unless otherwise specified.
Examples
Example 1
The embodiment discloses washable sun-proof emulsion and a preparation method thereof.
A washable sun-proof emulsion comprises the following raw materials: 120 parts of latex glue, 10 parts of compound vulcanizing agent, 4 parts of oleic acid and 1 part of linseed oil.
Wherein the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent and water, wherein the initiator is potassium persulfate, the dispersing agent is sodium methylene dinaphthyl sulfonate and polyoxyethylene stearate with the weight part ratio of 1:2, and the accelerator is accelerator M, accelerator ZDC and accelerator DPG with the weight part ratio of 4:4:1; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion comprises the following steps:
s1, preparing a composite vulcanizing agent; mixing and stirring 2-acetylamino-3-dimethylamino methyl acrylate, an initiator, a dispersing agent and 40 parts of water at normal temperature for 5 hours, blowing nitrogen for 2 hours, adding 7 parts of 2-ethylhexyl acrylate, stirring at 50 ℃ for 50 minutes, and dispersing at a rotating speed of 300r/min for 15 minutes; then adding the rest 2-ethylhexyl acrylate, and dispersing for 5min at the rotating speed of 300r/min to obtain an emulsion product; then adding sulfur, 2-hydroxy-4-methoxyl diphenyl ketone, an accelerator, ammonia water, detergent and the rest water, and continuously stirring for 4 hours;
s2, preparing a finished product; mixing the latex glue, the composite vulcanizing agent prepared in the step S1, oleic acid and linseed oil at the temperature of 30 ℃, stirring for 18 hours, and then foaming, injection molding and demolding to prepare the latex product.
Example 2
The embodiment discloses washable sun-proof emulsion and a preparation method thereof.
A washable sun-proof emulsion comprises the following raw materials: 130 parts of latex glue, 15 parts of compound vulcanizing agent, 6 parts of oleic acid and 2 parts of linseed oil.
Wherein the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent and water, wherein the initiator is potassium persulfate, the dispersing agent is sodium methylene dinaphthyl sulfonate and polyoxyethylene stearate with the weight part ratio of 1:2, and the accelerator is accelerator M, accelerator ZDC and accelerator DPG with the weight part ratio of 4:4:1; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion comprises the following steps:
s1, preparing a composite vulcanizing agent; mixing and stirring 2-acetylamino-3-dimethylamino methyl acrylate, an initiator, a dispersing agent and 50 parts of water at normal temperature for 6 hours, blowing nitrogen for 2 hours, adding 8 parts of 2-ethylhexyl acrylate, stirring at 60 ℃ for reaction for 60 minutes, and dispersing for 20 minutes at a rotating speed of 600 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 10min at the rotating speed of 600r/min to obtain an emulsion product; then adding sulfur, 2-hydroxy-4-methoxyl diphenyl ketone, an accelerator, ammonia water, detergent and the rest water, and continuously stirring for 5 hours;
s2, preparing a finished product; mixing the latex glue, the composite vulcanizing agent prepared in the step S1, oleic acid and linseed oil at the temperature of 32 ℃, stirring for 22 hours, and then foaming, injection molding and demolding to prepare the latex product.
Example 3
The embodiment discloses washable sun-proof emulsion and a preparation method thereof.
A washable sun-proof emulsion comprises the following raw materials: 125 parts of latex glue, 12 parts of compound vulcanizing agent, 5 parts of oleic acid and 2 parts of linseed oil.
Wherein the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent and water, wherein the initiator is potassium persulfate, the dispersing agent is sodium methylene dinaphthyl sulfonate and polyoxyethylene stearate with the weight part ratio of 1:2, and the accelerator is accelerator M, accelerator ZDC and accelerator DPG with the weight part ratio of 4:4:1; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion comprises the following steps:
s1, preparing a composite vulcanizing agent; mixing and stirring 2-acetylamino-3-dimethylamino methyl acrylate, an initiator, a dispersing agent and 45 parts of water at normal temperature for 5.5 hours, blowing nitrogen for 2 hours, adding 8 parts of acrylic acid-2-ethylhexyl ester, stirring and reacting for 55 minutes at 55 ℃, and dispersing for 18 minutes at a rotating speed of 450 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 8min at the rotating speed of 450r/min to obtain an emulsion product; then adding sulfur, 2-hydroxy-4-methoxyl diphenyl ketone, an accelerator, ammonia water, detergent and the rest water, and continuously stirring for 4.5 hours;
s2, preparing a finished product; mixing the latex glue, the composite vulcanizing agent prepared in the step S1, oleic acid and linseed oil at the temperature of 31 ℃, stirring for 20 hours, and then foaming, injection molding and demolding to prepare the latex product.
Example 4
The difference from example 1 is that the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent, water, 1, 2-propylenediamine, tert-butylcatechol, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, an antioxidant 616, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, wherein the initiator is potassium persulfate, the dispersing agent is 1:2 by weight of sodium methylenedinaphthyl sulfonate and polyoxyethylene stearate, the accelerator is 4:4:1 by weight of accelerator M, an accelerator ZDC and an accelerator DPG, and the catalyst is triethylamine; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion, S1 also comprises the following steps:
1, 2-propylene diamine, 2-acetylamino-3-dimethylaminomethyl acrylate and 8 parts of water are blended and stirred for 1h at 70 ℃ to obtain a mixture A; then, continuously adding an initiator, a dispersing agent and 40 parts of water into the mixture A, mixing and stirring for 5 hours at normal temperature, and blowing nitrogen for 2 hours, then adding 7 parts of 2-ethylhexyl acrylate, stirring and reacting for 50 minutes at 50 ℃, and dispersing for 15 minutes at a rotating speed of 300 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 5min at the rotating speed of 300r/min to obtain an emulsion product;
mixing tert-butylcatechol, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, and stirring and reacting for 50min at 50 ℃ to obtain a mixture B;
mixing the mixture B and the emulsion product and stirring for 30min; then adding sulfur, 2-hydroxy-4-methoxybenzophenone, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, antioxidant 616, accelerator, ammonia water, detergent and the rest water, and continuing stirring for 4-5 hours to prepare the compound vulcanizing agent.
Example 5
The difference from example 2 is that the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent, water, 1, 2-propylenediamine, tert-butylcatechol, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, an antioxidant 616, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, wherein the initiator is potassium persulfate, the dispersing agent is 1:2 by weight of sodium methylenedinaphthyl sulfonate and polyoxyethylene stearate, the accelerator is 4:4:1 by weight of accelerator M, an accelerator ZDC and an accelerator DPG, and the catalyst is triethylamine; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion, S1 also comprises the following steps:
1, 2-propylene diamine, 2-acetylamino-3-dimethylaminomethyl acrylate and 10 parts of water are blended and stirred for 1.5 hours at 80 ℃ to obtain a mixture A; then, continuously adding an initiator, a dispersing agent and 50 parts of water into the mixture A, mixing and stirring for 6 hours at normal temperature, and blowing nitrogen for 2 hours, then adding 8 parts of acrylic acid-2-ethylhexyl ester, stirring and reacting for 60 minutes at 60 ℃, and dispersing for 20 minutes at a rotating speed of 600 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 10min at the rotating speed of 600r/min to obtain an emulsion product;
mixing tert-butylcatechol, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, and stirring at 60 ℃ for reacting for 60min to obtain a mixture B;
mixing the mixture B and the emulsion product and stirring for 40min; then adding sulfur, 2-hydroxy-4-methoxybenzophenone, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, antioxidant 616, accelerator, ammonia water, detergent and the rest water, and continuously stirring for 5 hours to obtain the composite vulcanizing agent.
Example 6
The difference from example 3 is that the composite vulcanizing agent comprises the following components: sulfur, 2-ethylhexyl acrylate, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, 2-hydroxy-4-methoxybenzophenone, a dispersing agent, an accelerator, ammonia water, a detergent, water, 1, 2-propylenediamine, tert-butylcatechol, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, an antioxidant 616, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, wherein the initiator is potassium persulfate, the dispersing agent is 1:2 by weight of sodium methylenedinaphthyl sulfonate and polyoxyethylene stearate, the accelerator is 4:4:1 by weight of accelerator M, an accelerator ZDC and an accelerator DPG, and the catalyst is triethylamine; the contents of the components of the composite vulcanizing agent are shown in table 1 below.
A preparation method of washable sun-proof emulsion, S1 also comprises the following steps:
1, 2-propylene diamine, 2-acetylamino-3-dimethylaminomethyl acrylate and 9 parts of water are blended and stirred for 1.2h at 75 ℃ to obtain a mixture A; then, continuously adding an initiator, a dispersing agent and 45 parts of water into the mixture A, mixing and stirring for 5.5 hours at normal temperature, and blowing nitrogen for 2 hours, then adding 8 parts of 2-ethylhexyl acrylate, stirring and reacting for 55 minutes at 55 ℃, and dispersing for 18 minutes at a rotating speed of 450 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 8min at the rotating speed of 450r/min to obtain an emulsion product;
mixing tert-butylcatechol, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, and stirring and reacting for 55min at 55 ℃ to obtain a mixture B;
mixing the mixture B and the emulsion product and stirring for 35min; then adding sulfur, 2-hydroxy-4-methoxybenzophenone, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, antioxidant 616, accelerator, ammonia water, detergent and the rest water, and continuously stirring for 4.5 hours to prepare the compound vulcanizing agent.
Example 7
The difference from example 1 is that the components of the composite vulcanizing agent further include 1, 2-propanediamine, and the contents of the components of the composite vulcanizing agent are shown in the following table 2.
Example 8
The difference from example 7 is that 1, 2-propanediamine was replaced with adipic acid dihydrazide, and the contents of the respective components are shown in Table 2 below.
Example 9
The difference from example 1 is that the components of the composite vulcanizing agent further include t-butylcatechol, 2'- (2' -hydroxy-3 '-t-butyl-5' -methylphenyl) -5-chlorobenzotriazole, and antioxidant 616, the contents of each component of the composite vulcanizing agent being shown in table 2 below.
Example 10
The difference from example 9 is that the components of the composite vulcanizing agent also comprise sodium 4-methoxybenzaldehyde-3-sulfonate and triethylamine as catalyst, and the contents of the components of the composite vulcanizing agent are shown in the following table 2.
Example 11
The difference from example 10 is that tert-butylcatechol was replaced with butanol, and the contents of the respective components are shown in table 2 below.
Example 12
The difference from example 10 is that sodium 4-methoxybenzaldehyde-3-sulfonate was replaced with sodium phenylacetate, and the contents of the respective components are shown in Table 2 below.
Example 13
The difference from example 10 is that 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole and antioxidant 616 are replaced with antioxidant 1010.
Example 14
The difference from example 10 is that the catalyst triethylamine was replaced with dodecylbenzenesulfonic acid, and the contents of the components are shown in the following table 2.
Example 15
The difference from example 1 is that the initiator potassium persulfate is replaced by sodium bisulfite.
Comparative example
Comparative example 1
The difference from example 1 is that the complex vulcanizing agent is replaced with the same weight part of the vulcanizing agent DTDM.
Comparative example 2
The difference from example 1 is that 2-ethylhexyl acrylate is replaced by a polyethylene wax emulsion.
Comparative example 3
The difference from example 1 is that methyl 2-acetylamino-3-dimethylaminoacrylate is replaced by ethyl acetate.
Comparative example 4
The difference from example 1 is that 2-hydroxy-4-methoxybenzophenone is replaced with an antioxidant 1010.
Comparative example 5
The difference from example 1 is that the dispersant is replaced by laureth.
Comparative example 6
The difference from example 1 is that in the preparation method of washable sun-proof latex, 2-acetylamino-3-dimethylaminomethyl acrylate, an initiator, a dispersing agent and 40 parts of water are mixed and stirred for 5 hours at normal temperature, nitrogen is blown for 2 hours, 2-ethylhexyl acrylate is added, stirring reaction is carried out for 50 minutes at 50 ℃, and dispersion is carried out for 15 minutes at a rotating speed of 300r/min, so that an emulsion product is obtained; then adding sulfur, 2-hydroxy-4-methoxyl diphenyl ketone, an accelerator, ammonia water, detergent and the rest water, and continuously stirring for 4 hours.
Table 1 component content amounts of the composite vulcanizing agents of examples 1 to 6
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Sulfur, sulfur and its preparation method | 50 | 60 | 55 | 50 | 60 | 55 |
| 2-ethylhexyl acrylate | 10 | 12 | 11 | 10 | 12 | 11 |
| 2-Acetylamino-3-dimethylaminoacrylic acid methyl ester | 5 | 6 | 5 | 5 | 6 | 5 |
| Initiator(s) | 1 | 2 | 2 | 1 | 2 | 2 |
| 2-hydroxy-4-methoxybenzophenone | 3 | 4 | 3 | 3 | 4 | 3 |
| Dispersing agent | 6 | 9 | 8 | 6 | 9 | 8 |
| Accelerating agent | 36 | 45 | 40 | 36 | 45 | 40 |
| Ammonia water | 0.5 | 0.6 | 0.6 | 0.5 | 0.6 | 0.6 |
| Liquid detergent | 0.5 | 0.7 | 0.6 | 0.5 | 0.7 | 0.6 |
| Water and its preparation method | 120 | 130 | 125 | 120 | 130 | 125 |
| 1, 2-propanediamine | / | / | / | 1 | 2 | 2 |
| Tert-butylcatechol | / | / | / | 2 | 3 | 2 |
| 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole | / | / | / | 1 | 3 | 2 |
| Antioxidant 616 | / | / | / | 1 | 2 | 2 |
| 4-Methoxybenzaldehyde-3-sulfonic acid sodium salt | / | / | / | 4 | 5 | 5 |
| Catalyst | / | / | / | 0.4 | 0.6 | 0.5 |
Table 2 component content amounts of the composite vulcanizing agents of examples 7 to 14
| Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | Example 14 | |
| Sulfur, sulfur and its preparation method | 50 | 50 | 50 | 50 | 50 | 50 | 50 | 50 |
| 2-ethylhexyl acrylate | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
| 2-Acetylamino-3-dimethylaminoacrylic acid methyl ester | 5 | 5 | 5 | 5 | 5 | 5 | 5 | 5 |
| Initiator(s) | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| 2-hydroxy-4-methoxybenzophenone | 3 | 3 | 3 | 3 | 3 | 3 | 3 | 3 |
| Dispersing agent | 6 | 6 | 6 | 6 | 6 | 6 | 6 | 6 |
| Accelerating agent | 36 | 36 | 36 | 36 | 36 | 36 | 36 | 36 |
| Ammonia water | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Liquid detergent | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| Water and its preparation method | 120 | 120 | 120 | 120 | 120 | 120 | 120 | 120 |
| 1, 2-propanediamine/adipic acid dihydrazide | 1 | 1 | / | / | / | / | / | / |
| Tert-butylcatechol/butanol | / | / | 2 | 2 | 2 | 2 | 2 | 2 |
| 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole/antioxidant 1010 | / | / | 1 | 1 | 1 | 1 | 2 | 1 |
| Antioxidant 616 | / | / | 1 | 1 | 1 | 1 | / | 1 |
| Sodium 4-methoxybenzaldehyde-3-sulfonate/sodium phenylacetate | / | / | / | 4 | 4 | 4 | 4 | 4 |
| Catalyst | / | / | / | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
Performance test
(1) Appearance test: characterized by gray scale and appearance change; photo-aging test is carried out on the latex samples prepared in the examples 1-6, and the latex samples are irradiated by a xenon lamp, and the test standard of GB/T250-2008 is combined with reference to ISO 4892-2:2013; irradiance of: (0.51+ -0.2) W/(m2.nm) @340nm, light: 102min, black mark temperature: (65+ -2) deg.C, box temperature: (38+ -2) deg.C, relative humidity: (50±10)% RH, exposure time: 300h.
According to GB/T250-2008, in the application, the gray scale grade is evaluated under a standard light source D65, the grade 5 is the best, the grade 1 is the worst, and the appearance change is qualified if no chalking exists; the appearance test results of examples 1-6 are shown in FIGS. 1-2, and the gray scale level and appearance change results are shown in Table 3 below.
(2) Sun protection performance test: sun protection performance T (UVA) AV Value characterization, T (UVA) AV The value is the arithmetic mean of the transmittance of solar ultraviolet radiation UVA at a wavelength of 315-400 nm; reference is made to the specification of the GB/T18830-2009 standard, when T (UVA) is the product AV When the value is less than 5%, which may be referred to as "ultraviolet shielding product", initial T (UVA) of the latex samples prepared in each of examples and comparative examples is measured AV A value; the latex samples prepared in examples 1 to 6 and comparative example 1 were washed 30 times again, respectively, and T (UVA) was measured again AV Values, test results are shown in table 4 below.
Table 3 table of appearance test results for examples 1-6
| Gray scale | Appearance change | |
| Example 1 | 2 | Visible yellowing, hardening and scorching, no visible chalking |
| Example 2 | 2 | Visible yellowing, hardening and scorching, no visible chalking |
| Example 3 | 2 | Visible yellowing, hardening and scorching, no visible chalking |
| Example 4 | 3 | Visible yellowing, cracking and hardening, no visible chalking |
| Example 5 | 3 | Visible yellowing, cracking and hardening, no visible chalking |
| Example 6 | 3 | Visible yellowing, cracking and hardening, no visible chalking |
Therefore, the latex product prepared by the technical scheme of the application has better sun-proof performance.
Table 4 results of the sunscreen performance test of each of the examples and comparative examples
| Initial T (UVA) AV /% | T after 30 washes (UVA) AV /% | |
| Example 1 | 4.40 | 4.94 |
| Example 2 | 4.01 | 4.62 |
| Example 3 | 4.22 | 4.78 |
| Example 4 | 1.66 | 2.15 |
| Example 5 | 1.20 | 1.74 |
| Example 6 | 1.41 | 1.95 |
| Example 7 | 3.42 | / |
| Example 8 | 3.68 | / |
| Example 9 | 3.07 | / |
| Example 10 | 2.75 | / |
| Example 11 | 3.25 | / |
| Example 12 | 3.29 | / |
| Example 13 | 2.88 | / |
| Example 14 | 2.85 | / |
| Example 15 | 4.45 | / |
| Comparative example 1 | 32.04 | 38.87 |
| Comparative example 2 | 8.97 | / |
| Comparative example 3 | 8.43 | / |
| Comparative example 4 | 5.05 | / |
| Comparative example 5 | 4.60 | / |
| Comparative example 6 | 7.13 | / |
In conclusion, the latex prepared by the technical scheme of the application has lower T (UVA) AV The latex disclosed by the application still has good sun-proof performance after being washed for many times, so that the latex product can be sterilized by long-time irradiation of sunlight better after being washed, and the service life is longer.
The present embodiment is merely for explaining the present application and does not limit the scope of the present application in this way, and a person skilled in the art can make modifications to the present embodiment without creative contribution as required after reading the present specification, but is protected by patent law only within the scope of the claims of the present application.
Claims (6)
1. A washable sun-proof emulsion, characterized in that: the material comprises the following raw materials in parts by weight:
120-130 parts of latex glue;
10-15 parts of a composite vulcanizing agent;
4-6 parts of oleic acid;
1-2 parts of linseed oil;
the composite vulcanizing agent comprises the following components in parts by weight:
50-60 parts of sulfur;
10-12 parts of 2-ethylhexyl acrylate;
5-6 parts of 2-acetylamino-3-dimethylaminomethyl acrylate;
1-2 parts of an initiator;
10-15 parts of 2-hydroxy-4-methoxybenzophenone;
6-9 parts of dispersing agent;
36-45 parts of an accelerator;
0.5-0.6 part of ammonia water;
0.5-0.7 part of detergent;
120-130 parts of water;
1-2 parts of 1, 2-propylene diamine;
2-3 parts of tert-butylcatechol;
1-3 parts of 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole;
1-2 parts of an antioxidant 616;
4-5 parts of sodium 4-methoxybenzaldehyde-3-sulfonate;
0.4-0.6 part of catalyst;
the preparation method of the composite vulcanizing agent comprises the following steps:
blending 1, 2-propylene diamine, 2-acetylamino-3-dimethylaminomethyl acrylate and 8-10 parts of water, and stirring at 70-80 ℃ for 1-1.5h to obtain a mixture A; then continuously adding an initiator, a dispersing agent and 40-50 parts of water into the mixture A, mixing and stirring for 5-6 hours at normal temperature, and blowing nitrogen for 2 hours, then adding 7-8 parts of 2-ethylhexyl acrylate, stirring and reacting for 50-60 minutes at 50-60 ℃, and dispersing for 15-20 minutes at a rotating speed of 300-600 r/min; then adding the rest 2-ethylhexyl acrylate, and dispersing for 5-10min at the rotating speed of 300-600r/min to obtain an emulsion product;
mixing tert-butylcatechol, 4-methoxybenzaldehyde-3-sodium sulfonate and a catalyst, and stirring at 50-60 ℃ for reacting for 50-60min to obtain a mixture B;
mixing the mixture B and the emulsion product and continuously stirring for 30-40min; then adding sulfur, 2-hydroxy-4-methoxybenzophenone, 2'- (2' -hydroxy-3 '-tert-butyl-5' -methylphenyl) -5-chlorobenzotriazole, antioxidant 616, accelerator, ammonia water, detergent and the rest of water, and continuing stirring for 4-5 hours.
2. A washable sunscreen emulsion according to claim 1, wherein: the catalyst is triethylamine.
3. A washable sunscreen emulsion according to claim 1, wherein: the initiator is potassium persulfate.
4. A washable sunscreen emulsion according to claim 1, wherein: the dispersing agent comprises sodium methylene dinaphthyl sulfonate and polyoxyethylene stearate, and the weight ratio of the sodium methylene dinaphthyl sulfonate to the polyoxyethylene stearate is 1:2.
5. A washable sunscreen emulsion according to claim 1, wherein: the accelerator comprises an accelerator M, an accelerator ZDC and an accelerator DPG, and the accelerator M is prepared from the following components in parts by weight: promoter ZDC: accelerator dpg=4:4:1.
6. A method of preparing a washable, sun-blocking emulsion as defined in claim 1, comprising the steps of:
s1, preparing a composite vulcanizing agent;
s2, preparing a finished product; mixing the latex glue, the composite vulcanizing agent prepared in the step S1, oleic acid and linseed oil at the temperature of 30-32 ℃, stirring for 18-22 hours, and then foaming, injection molding and demolding to prepare the latex product.
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