CN112409554A - Environment-friendly natural latex and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of preparation of latex materials, in particular to environment-friendly natural latex and a preparation method thereof; according to the invention, firstly, an allyl chlorosilane compound is grafted to a natural latex molecular chain under an alkaline condition, and then a free radical crosslinking reaction is carried out in a double-bond modified chitosan solution under the action of an initiator, so that the crosslinking density of the natural latex can be increased, the double-bond content in molecules is consumed, the solvent resistance of a natural latex product is improved, and the aging resistance of the product is improved; the natural latex of the invention modifies the molecular chain of the latex through the natural modified chitosan, thereby achieving the purposes of improving the defects of the natural latex and improving the quality of the natural latex product.
Description
Technical Field
The invention relates to the field of preparation of latex materials, in particular to environment-friendly natural latex and a preparation method thereof.
Background
The natural latex is a natural resource which is synthesized by biology and can be regenerated, and has excellent physical and mechanical properties.
CN106750611A discloses a modified natural latex material, which comprises the following components in percentage by weight: 0.2-5% of silk fibroin, 0.05-2% of silicon dioxide, 0.1-2% of polymethyl methacrylate, 0.05-1% of resorcinol bis (diphenyl) phosphate and the balance of natural latex. The emulsion film prepared by the emulsion material has greatly improved mechanical property and solvent resistance.
CN102977423A A method for modifying natural latex with waterborne polyurethane comprises the steps of preparing a prepolymer by taking IPDI, PTMG, BDO and DMPA as raw materials, adding HEA to carry out end capping on end-NCO of the prepolymer, reacting for 50min, cooling to 40 ℃, adding triethylamine to carry out neutralization reaction to generate salt, reacting for 3-4min, adding water to emulsify for 60min, and obtaining waterborne polyurethane emulsion; and physically blending the waterborne polyurethane and the natural latex to obtain the waterborne polyurethane modified natural latex. The waterborne polyurethane modified natural latex obtained by the invention can improve the smoothness, compactness and mechanical strength of a natural latex film and simultaneously reduce the escape of allergenic protein.
CN105906854A discloses a method for modifying a graphene-modified natural latex polymer, which comprises modifying graphene with a coupling agent, and then uniformly dispersing the modified functionalized graphene in natural rubber, so as to solve the problem of non-uniform dispersion of graphene in natural rubber and obtain modified natural rubber; the mechanical property of the graphene modified natural latex polymer obtained by the method is improved by 20-200%, the barrier property is improved, various viruses can be blocked, and the raw materials adopted by the graphene modified natural latex polymer modification method are easy to obtain and are easy for large-scale production. The invention also discloses a graphene modified natural latex polymer prepared by the method.
In the production process of the latex, biological organisms can secrete substances such as proteins, fatty acids, saccharides and the like to be mixed into the latex, so that the latex generates anaphylactic reaction on a human body, and the problems of poor solvent resistance and poor ageing resistance of a latex product are caused.
Disclosure of Invention
In order to solve the problems, the invention provides an environment-friendly natural latex and a preparation method thereof.
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
according to the mass parts, adding 0.1-0.8 part of 10-20% sodium hydroxide solution into 120 parts of 100-0.8 parts of natural latex, stirring and mixing uniformly, slowly adding 3.8-6.2 parts of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 1-5h to obtain propenyl silane grafted natural latex; then adding 0.1-0.5 part of initiator into the latex, uniformly mixing, controlling the temperature to 50-75 ℃, then slowly adding 55-75 parts of double-bond modified chitosan solution into the reaction kettle, finishing the addition within 30-60min, supplementing 0.05-0.1 part of initiator after the completion, controlling the temperature to 50-70 ℃, reacting for 120-180min, then cooling to room temperature, and continuously stirring for 1-5h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
according to the mass portion of the raw materials,
1) adding 5-10 parts of chitosan into 60-100 parts of sodium acetate-acetic acid solution with the pH value of 4.2-4.8, stirring and mixing uniformly, bubbling the solution for 5-30min by using inert gas, then keeping the temperature of the solution at-5-5 ℃, dissolving 0.5-1.8 parts of potassium periodate into 5-10 parts of sodium acetate-acetic acid solution with the pH value of 4.2-4.8, slowly adding the solution into a reaction kettle, controlling the solution to be added within 10-30min, then heating to room temperature, reacting for 10-24h under the condition of light shielding, then adding 0.8-2.4 parts of ethylene glycol to stop the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 30-50 parts of 1) oxidized chitosan into 30 parts of 0.1-5% sodium hydroxide solution for dispersion, then adding 3-10 parts of hydroxyethyl acrylate, 0.5-1 part of allyl alcohol, 0.05-0.1 part of-hydroxyethyl-3-methylimidazolium tetrafluoroborate (CAS:374564-83-7) and 0.05-0.5 part of 2-hydroxymethyl-12-crown ether-4, heating to 40-80 ℃, reacting for 4-12h, cooling to normal temperature, and adding acetic acid until the pH value is 6-8 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 85% -90%.
The main synthesis mode of the double-bond modified chitosan solution can be expressed as follows:
the allyl chlorosilane compound is allyl (chloromethyl) dimethylsilane or allyl dimethylchlorosilane.
The initiator is azodiisobutyronitrile or benzoyl peroxide.
According to the environment-friendly natural latex and the preparation method thereof, firstly, an allyl chlorosilane compound is grafted to a natural latex molecular chain under an alkaline condition, and then, a double-bond modified chitosan solution is subjected to a free radical crosslinking reaction under the action of an initiator, so that the crosslinking density of the natural latex can be increased, the double-bond content in molecules is consumed, and the solvent resistance of a natural latex product is improved; during the reaction process, the residual aldehyde group and other polar side groups in the oxidized chitosan interact with a small amount of proteins, fatty acids, saccharides and other substances in the latex, and in the process of curing and film-forming the latex, the imidazole tetrafluoroborate and crown ether which are non-rubber substances migrate and gather to the surface of the film to form an oil-resistant protective film on the surface of the latex film, so that the solvent resistance of the modified latex film is increased, and the aging resistance of the product is improved; the natural latex of the invention modifies the molecular chain of the latex through the natural modified chitosan, thereby achieving the purposes of improving the defects of the natural latex and improving the quality of the natural latex product.
Drawings
FIG. 1 is a Fourier infrared spectrum of the eco-friendly natural latex prepared in example 2:
at 2918cm-1An absorption peak of a carbon-hydrogen bond exists nearby, which indicates that the natural latex participates in the reaction; at 1072cm-1An absorption peak of ether bond at 3335/1476cm is present in the vicinity thereof-1The expansion/in-plane bending absorption peak of hydroxyl exists nearby and is 1017cm-1An absorption peak of a carbon-nitrogen single bond exists nearby, which indicates that the double-bond modified chitosan participates in the reaction; at 771cm-1A stretching absorption peak of silicon-carbon bond exists nearby, so that the allyl chlorosilane participates in the reaction.
Detailed Description
The invention is further illustrated by the following specific examples:
the natural latex prepared in the following examples and comparative examples is defoamed, poured into a polystyrene culture dish, and dried into a film for 12 hours at 70 ℃ by a solution casting method to prepare the modified latex film.
Cutting a latex film sample to be tested into dumbbell-shaped sample strips with the test length of 20mm and the test width of 4mm by using a 2-type cutter, measuring the thicknesses of 5 different positions on a sample strip test area, averaging, standing for 24 hours, measuring the tensile strength and the elongation at break of the latex film on a Zwick/Roell Z020 type electronic universal tensile testing machine according to a GB/T528-2009 method, measuring each group of samples for 5 times, and averaging. And (3) testing conditions are as follows: the drawing rate was 200mm/min, the temperature was 20 ℃ and the relative humidity was 40%.
The latex film was tested for solvent resistance in toluene according to GB/T1690-92. Preparing a sample of the latex film to be detected into a size of 25mm multiplied by 25mm at 25 ℃, soaking the sample in methylbenzene for 24 hours, taking out the solvent on the surface of the wiped film, weighing the solvent, putting the latex film in an oven, drying for 6 hours, and weighing the dried latex film. The solvent resistance of the latex film was measured by the change in mass of the latex film.
Example 1
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 0.1g of 10% sodium hydroxide solution in parts by mass into 100g of natural latex, stirring and mixing uniformly, slowly adding 3.8g of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 1 hour to obtain propenyl silane grafted natural latex; and then adding 0.1g of initiator into the latex, uniformly mixing, controlling the temperature to 50 ℃, slowly adding 55g of double-bond modified chitosan solution into the reaction kettle, adding 0.05g of initiator after finishing the addition within 30min, controlling the temperature to 50 ℃, reacting for 120min, cooling to room temperature, and continuously stirring for 1h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
1) adding 10g of chitosan into 100g of sodium acetate-acetic acid solution with the pH value of 4.2, uniformly stirring and mixing, bubbling the solution for 30min by using inert gas, then keeping the temperature of the solution at 5 ℃, dissolving 1.8g of potassium periodate into 10g of sodium acetate-acetic acid solution with the pH value of 4.2, slowly adding the solution into a reaction kettle, controlling the solution to be added for 30min, then heating to room temperature, reacting for 10h in a dark condition, then adding 2.4g of ethylene glycol to terminate the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 50g of 1) oxidized chitosan into 30g of 5% sodium hydroxide solution for dispersion, then adding 10g of hydroxyethyl acrylate, 0.5g of allyl alcohol, 0.1g of hydroxyethyl-3-methylimidazolium tetrafluoroborate CAS:374564-83-7 and 0.5g of 2-hydroxymethyl-12-crown ether-4, heating to 80 ℃ for reaction for 4 hours, then cooling to normal temperature, and adding acetic acid until the pH value is 8 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 90%.
The propenyl chlorosilane compound is propenyl (chloromethyl) dimethylsilane.
The initiator is azodiisobutyronitrile.
Example 2
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 0.4g of sodium hydroxide solution with the mass part of 15% into 110g of natural latex, stirring and mixing uniformly, slowly adding 5.2g of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 2 hours to obtain propenyl silane grafted natural latex; and then adding 0.2g of initiator into the latex, uniformly mixing, controlling the temperature to 65 ℃, slowly adding 65g of double-bond modified chitosan solution into the reaction kettle, adding 0.08g of initiator within 45min, controlling the temperature to be 60 ℃, reacting for 150min, cooling to room temperature, and continuously stirring for 3h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
1) adding 5g of chitosan into 60g of sodium acetate-acetic acid solution with the pH value of 4.8, stirring and mixing uniformly, bubbling the solution for 5min by using inert gas, then keeping the temperature of the solution at-5 ℃, then dissolving 0.5g of potassium periodate into 5g of sodium acetate-acetic acid solution with the pH value of 4.8, slowly adding the solution into a reaction kettle, controlling the solution to be added for 10min, then heating to room temperature, reacting for 24h under the condition of light shielding, then adding 0.8g of ethylene glycol to terminate the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 30g of 1) oxidized chitosan into 30g of 0.1% sodium hydroxide solution for dispersion, then adding 3g of hydroxyethyl acrylate, 1g of allyl alcohol, 0.05g of hydroxyethyl-3-methylimidazolium tetrafluoroborate CAS:374564-83-7 and 0.05g of 2-hydroxymethyl-12-crown ether-4, heating to 40 ℃ for reaction for 12 hours, then cooling to normal temperature, and adding acetic acid until the pH value is 6 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 85%.
The allyl chlorosilane compound is allyl dimethyl chlorosilane.
The initiator is benzoyl peroxide.
Example 3
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 0.8g of 20% sodium hydroxide solution in parts by mass into 120g of natural latex in parts by mass, uniformly stirring and mixing, slowly adding 6.2g of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 5 hours to obtain propenyl silane grafted natural latex; and then adding 0.5g of initiator into the latex, uniformly mixing, controlling the temperature to 75 ℃, slowly adding 75g of double-bond modified chitosan solution into the reaction kettle, adding 0.1g of initiator after finishing the addition within 60min, controlling the temperature to 70 ℃, reacting for 180min, cooling to room temperature, and continuously stirring for 5h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
1) adding 8g of chitosan into 80g of sodium acetate-acetic acid solution with the pH value of 4.5, stirring and mixing uniformly, bubbling the solution for 20min by using inert gas, then keeping the temperature of the solution at 0 ℃, dissolving 1.2g of potassium periodate into 7g of sodium acetate-acetic acid solution with the pH value of 4.5, slowly adding the solution into a reaction kettle, controlling the solution to be added for 20min, then heating to room temperature, reacting for 18h in a dark condition, then adding 1.6g of ethylene glycol to terminate the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 40g of 1) oxidized chitosan into 30 parts of 2% sodium hydroxide solution for dispersion, then adding 7g of hydroxyethyl acrylate, 0.7g of allyl alcohol, 0.6g of hydroxyethyl-3-methylimidazolium tetrafluoroborate CAS:374564-83-7 and 0.3g of 2-hydroxymethyl-12-crown ether-4, heating to 65 ℃ for reaction for 9 hours, then cooling to normal temperature, and adding acetic acid until the pH value is 7 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 87%.
The allyl chlorosilane compound is allyl dimethyl chlorosilane.
The initiator is benzoyl peroxide.
The quality test data of the reclaimed rubber prepared by the above example are shown in the following table:
| tensile Strength (MPa) | Elongation at Break (%) | Weight loss (%) | |
| Example 1 | 24.61 | 872 | 1.86 |
| Example 2 | 26.27 | 924 | 1.42 |
| Example 3 | 26.93 | 951 | 1.34 |
Comparative example 1
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 0.1g of initiator into 100g of natural latex according to the mass portion, uniformly mixing, controlling the temperature to 50 ℃, slowly adding 55g of double-bond modified chitosan solution into a reaction kettle, finishing the addition within 30min, supplementing 0.05g of initiator after the completion, controlling the temperature to 50 ℃, reacting for 120min, cooling to room temperature, and continuously stirring for 1h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
1) adding 10g of chitosan into 100g of sodium acetate-acetic acid solution with the pH value of 4.2, uniformly stirring and mixing, bubbling the solution for 30min by using inert gas, then keeping the temperature of the solution at 5 ℃, dissolving 1.8g of potassium periodate into 10g of sodium acetate-acetic acid solution with the pH value of 4.2, slowly adding the solution into a reaction kettle, controlling the solution to be added for 30min, then heating to room temperature, reacting for 10h in a dark condition, then adding 2.4g of ethylene glycol to terminate the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 50g of 1) oxidized chitosan into 30g of 5% sodium hydroxide solution for dispersion, then adding 10g of hydroxyethyl acrylate, 0.5gg of allyl alcohol, 0.1g of hydroxyethyl-3-methylimidazole tetrafluoroborate CAS:374564-83-7 and 0.5g of 2-hydroxymethyl-12-crown ether-4, heating to 80 ℃ for reaction for 4 hours, then cooling to the normal temperature, and adding acetic acid until the pH value is 8 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 90%.
The initiator is azodiisobutyronitrile.
Comparative example 2
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 0.1g of sodium hydroxide solution with the mass g of 10% into 100g of natural latex, stirring and mixing uniformly, slowly adding 3.8g of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 1 hour to obtain propenyl silane grafted natural latex; and then adding 0.1g of initiator into the latex, uniformly mixing, controlling the temperature to 50 ℃, slowly adding 55g of chitosan solution into the reaction kettle, adding 0.05g of initiator within 30min, controlling the temperature to 50 ℃, reacting for 120min, cooling to room temperature, and continuously stirring for 1h to obtain the environment-friendly natural latex.
The preparation method of the chitosan solution comprises the following steps:
adding 8g of chitosan into 45g of 1.5% hydrochloric acid solution, uniformly mixing, controlling the temperature to be 65 ℃, and stirring for 60min to obtain the chitosan solution.
The propenyl chlorosilane compound is propenyl (chloromethyl) dimethylsilane.
The initiator is azodiisobutyronitrile.
Comparative example 3
An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
adding 3.8g of allyl chlorosilane compound into 100g of natural latex, slowly adding the natural latex into a reaction kettle, and stirring for reaction for 1 hour to obtain allyl silane grafted natural latex; and then adding 0.1g of initiator into the latex, uniformly mixing, controlling the temperature to 50 ℃, slowly adding 55g of double-bond modified chitosan solution into the reaction kettle, adding 0.05g of initiator after finishing the addition within 30min, controlling the temperature to 50 ℃, reacting for 120min, cooling to room temperature, and continuously stirring for 1h to obtain the environment-friendly natural latex.
The preparation method of the double-bond modified chitosan solution comprises the following steps:
1) adding 10g of chitosan into 100g of sodium acetate-acetic acid solution with the pH value of 4.2, uniformly stirring and mixing, bubbling the solution for 30min by using inert gas, then keeping the temperature of the solution at 5 ℃, dissolving 1.8g of potassium periodate into 10g of sodium acetate-acetic acid solution with the pH value of 4.2, slowly adding the solution into a reaction kettle, controlling the solution to be added for 30min, then heating to room temperature, reacting for 10h in a dark condition, then adding 2.4g of ethylene glycol to terminate the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 50g of 1) oxidized chitosan into 30g of 5% sodium hydroxide solution for dispersion, then adding 10g of hydroxyethyl acrylate, 0.5gg of allyl alcohol, 0.1g of hydroxyethyl-3-methylimidazole tetrafluoroborate CAS:374564-83-7 and 0.5g of 2-hydroxymethyl-12-crown ether-4, heating to 80 ℃ for reaction for 4 hours, then cooling to the normal temperature, and adding acetic acid until the pH value is 8 to obtain the double-bond modified chitosan solution.
The inert gas is high-purity nitrogen with the content of more than 99.999 percent.
The deacetylation degree of the chitosan is 90%.
The propenyl chlorosilane compound is propenyl (chloromethyl) dimethylsilane.
The initiator is azodiisobutyronitrile.
The quality test data of the reclaimed rubber prepared by the above example are shown in the following table:
| tensile Strength (MPa) | Elongation at Break (%) | Weight loss (%) | |
| Comparative example 1 | 18.42 | 712 | 5.82 |
| Comparative example 2 | 19.37 | 749 | 5.14 |
| Comparative example 3 | 22.17 | 816 | 3.47 |
Claims (6)
1. An environment-friendly natural latex and a preparation method thereof, the specific scheme is as follows:
according to the mass parts, adding 0.1-0.8 part of 10-20% sodium hydroxide solution into 120 parts of 100-0.8 parts of natural latex, stirring and mixing uniformly, slowly adding 3.8-6.2 parts of propenyl chlorosilane compound into a reaction kettle, and stirring and reacting for 1-5h to obtain propenyl silane grafted natural latex; then adding 0.1-0.5 part of initiator into the latex, uniformly mixing, controlling the temperature to 50-75 ℃, then slowly adding 55-75 parts of double-bond modified chitosan solution into the reaction kettle, finishing the addition within 30-60min, supplementing 0.05-0.1 part of initiator after the completion, controlling the temperature to 50-70 ℃, reacting for 120-180min, then cooling to room temperature, and continuously stirring for 1-5h to obtain the environment-friendly natural latex.
2. The environmental-friendly natural latex and the preparation method thereof as claimed in claim 1, wherein: the preparation method of the double-bond modified chitosan solution comprises the following steps: according to the mass portion of the raw materials,
1) adding 5-10 parts of chitosan into 60-100 parts of sodium acetate-acetic acid solution with the pH value of 4.2-4.8, stirring and mixing uniformly, bubbling the solution for 5-30min by using inert gas, then keeping the temperature of the solution at-5-5 ℃, dissolving 0.5-1.8 parts of potassium periodate into 5-10 parts of sodium acetate-acetic acid solution with the pH value of 4.2-4.8, slowly adding the solution into a reaction kettle, controlling the solution to be added within 10-30min, then heating to room temperature, reacting for 10-24h under the condition of light shielding, then adding 0.8-2.4 parts of ethylene glycol to stop the reaction, pouring the reaction solution into ethanol for precipitation, and obtaining oxidized chitosan containing aldehyde groups;
2) adding 30-50 parts of 1) oxidized chitosan into 30 parts of 0.1-5% sodium hydroxide solution for dispersion, then adding 3-10 parts of hydroxyethyl acrylate, 0.5-1 part of allyl alcohol, 0.05-0.1 part of-hydroxyethyl-3-methylimidazole tetrafluoroborate and 0.05-0.5 part of 2-hydroxymethyl-12-crown ether-4, heating to 40-80 ℃, reacting for 4-12h, cooling to normal temperature, and adding acetic acid until the pH value is 6-8 to obtain the double-bond modified chitosan solution.
3. The environmental-friendly natural latex and the preparation method thereof as claimed in claim 2, wherein: the inert gas is high-purity nitrogen with the content of more than 99.999 percent.
4. The environmental-friendly natural latex and the preparation method thereof as claimed in claim 2, wherein: the deacetylation degree of the chitosan is 85% -90%.
5. The environmental-friendly natural latex and the preparation method thereof as claimed in claim 1, wherein: the allyl chlorosilane compound is allyl (chloromethyl) dimethylsilane or allyl dimethylchlorosilane.
6. The environmental-friendly natural latex and the preparation method thereof as claimed in claim 1, wherein: the initiator is azodiisobutyronitrile or benzoyl peroxide.
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