CN113045726A - High-molecular antibacterial polyurethane memory cotton and preparation method thereof - Google Patents
High-molecular antibacterial polyurethane memory cotton and preparation method thereof Download PDFInfo
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- CN113045726A CN113045726A CN202110525377.9A CN202110525377A CN113045726A CN 113045726 A CN113045726 A CN 113045726A CN 202110525377 A CN202110525377 A CN 202110525377A CN 113045726 A CN113045726 A CN 113045726A
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- antibacterial
- polyether polyol
- polyurethane memory
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- memory cotton
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4833—Polyethers containing oxyethylene units
- C08G18/4837—Polyethers containing oxyethylene units and other oxyalkylene units
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4081—Mixtures of compounds of group C08G18/64 with other macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4829—Polyethers containing at least three hydroxy groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2280/00—Compositions for creating shape memory
Abstract
The invention relates to a macromolecule antibacterial polyurethane memory cotton and a preparation method thereof, wherein the macromolecule antibacterial polyurethane memory cotton is prepared by taking a poly-guanidine modified isocyanate prepolymer, a polyether polyol I, a polyether polyol II, a foam stabilizer and a compound amine catalyst as raw materials, and permanently grafting an antibacterial group on a polyurethane chain segment in the poly-guanidine modified isocyanate prepolymer, so that the prepared macromolecule antibacterial polyurethane memory cotton has good environmental security and lasting antibacterial performance, and effectively solves the problems of antibacterial performance reduction and pollution caused by the migration of an antibacterial agent in the prior art by adopting an additional blending type antibacterial polyurethane. The data show that the antibacterial rate of the obtained macromolecular antibacterial polyurethane memory cotton is up to 99% according to the national standard GB/T20944, and the antibacterial rate is up to 98.5% after 50 times of water washing.
Description
Technical Field
The invention belongs to the technical field of polyurethane materials, and particularly relates to high-molecular antibacterial polyurethane memory cotton and a preparation method thereof.
Background
The polyurethane memory cotton belongs to one of polyurethane materials, is a multi-block copolymer, has a relatively excellent thermotropic shape memory function, and has the commonality of plastics and rubber. The polyurethane memory cotton mainly comprises soft-segment high polymer with low thermal transition temperature and hard-segment high polymer with high thermal transition temperature, wherein the soft-segment high polymer is generally composed of polyester or polyether polyol and is a reversible phase, and the hard-segment high polymer is composed of carbamate chain segment molecules through extremely strong hydrogen bond interaction and is a stationary phase. Due to the difference of the molecular structures of the soft segment and the hard segment in the polyurethane, the soft segment and the hard segment have incompatibility in thermodynamics, microphase separation is generated, and the thermal transition temperatures of the soft segment and the hard segment are different, so that the polyurethane has a shape memory function at a certain temperature. The shape recovery temperature is adjusted by selecting and proportioning the raw materials, and the polyurethane memory cotton material with different memory temperatures can be obtained.
Polyurethane memory cotton is commonly used in daily life occasions of people, such as mattresses, pillows, sofas and the like. After long-term use, dander, sweat stain and the like are retained in pores of the polyurethane foam, and bacteria are easy to grow. Therefore, the antibacterial performance of the material is improved, and the method is very significant. The antibacterial agent can be classified into an inorganic antibacterial agent and an organic antibacterial agent according to the difference of the constituent elements of the antibacterial agent. The inorganic antibacterial agent comprises nano silver, copper, titanium dioxide, zinc oxide and the like, the organic antibacterial agent comprises natural antibacterial materials such as polysaccharide, polypeptide, chitosan and the like, and synthetic organic antibacterial materials such as antibiotics, quaternary ammonium salt, guanidine compounds and the like. The prior art mostly achieves the antibacterial effect by additionally adding an antibacterial agent. The invention patent CN111440283A improves the antibacterial effect of the memory cotton through the synergistic effect of the nano silver and the far infrared additive, and the invention patent CN105400176A improves the antibacterial effect through the compounding of the organic antibacterial agent, the nano silver antibacterial agent and the chitosan, but is still an external blending mode in essence, and is easy to migrate to cause the reduction of the antibacterial performance and environmental pollution.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a high-molecular antibacterial polyurethane memory cotton and a preparation method thereof. According to the invention, the organic polymer antibacterial agent is reacted with isocyanate in advance, so that the antibacterial group is permanently grafted on the polyurethane chain segment, and the memory cotton material which is environment-friendly, safe and has a lasting antibacterial property is obtained.
The technical scheme adopted by the invention is as follows:
a high-molecular antibacterial polyurethane memory cotton comprises the following raw material components:
30-60 parts of polyguanidine modified isocyanate prepolymer;
55-85 parts of polyether polyol I;
15-40 parts of polyether polyol II;
0.5-2 parts by weight of foam stabilizer;
0.5-1.5 parts by weight of composite amine catalyst;
2-4 parts of water.
The polyguanidine modified isocyanate prepolymer is prepared by the following method:
(S1) dissolving polyhexamethylene biguanide hydrochloride in polyether polyol I to obtain a mixture;
(S2) dropwise adding the mixture obtained in the step (S1) into isocyanate under the condition of heating and stirring, continuously reacting for a period of time at constant temperature after dropwise adding, and cooling to obtain the polyguanidine modified isocyanate prepolymer.
In the step (S1), the molecular formula of polyhexamethylene biguanide hydrochloride is (C)8H17N5)nxHCl, n is a natural number between 12 and 16, and the addition amount of the polyhexamethylene biguanide hydrochloride accounts for 10 percent of the mass of the polyether polyol I;
the polyether polyol I is ethylene oxide propylene oxide copolymerized polyether polyol, wherein the EO content is more than or equal to 50%, the molecular weight is 3500-5000, the functionality is 3-4, the primary hydroxyl end capping is more than or equal to 80%, and the moisture content is less than or equal to 0.05%.
In the step (S2), the mass ratio of the mixture to the isocyanate is 1:5, the heating temperature is 80 ℃, and the dropping time is 1 h.
After the addition was complete, the reaction was continued at 80 ℃ for 1 h.
In the step (S2), the isocyanate is one or more of pure MDI, crude MDI and polyol modified MDI, and the NCO content of the isocyanate is 25.5-33.6%.
The polyether polyol II is slow rebound polyether, the functionality is 3-4, the molecular weight is 500-1000, and the hydroxyl value is 160-340.
The foam stabilizer is polyether modified organic siloxane.
The composite amine catalyst is one or more of dimethylethanolamine, bis (dimethylaminoethyl) ether, triethylenediamine and triethylenediamine;
the composite amine catalyst is a closed delayed catalyst or a reaction catalyst.
The preparation method of the macromolecular antibacterial polyurethane memory cotton comprises the following steps:
(1) respectively taking polyether polyol I, polyether polyol II, a foam stabilizer, a composite amine catalyst and water, and fully mixing and stirring uniformly at room temperature to obtain a combined material;
(2) and (2) adding the polyguanidine modified isocyanate prepolymer into the combined material obtained in the step (1), fully and uniformly mixing, and forming and curing to obtain the high-molecular antibacterial polyurethane memory cotton.
The invention has the beneficial effects that:
according to the macromolecular antibacterial polyurethane memory cotton, the polyguanidine-modified isocyanate prepolymer, the polyether polyol I, the polyether polyol II, the foam stabilizer and the compound amine catalyst are used as raw materials, and the antibacterial group in the polyguanidine-modified isocyanate prepolymer is permanently grafted on the polyurethane chain segment, so that the prepared macromolecular antibacterial polyurethane memory cotton is good in environmental safety and has a lasting antibacterial property, and the problems of antibacterial performance reduction and pollution caused by the migration of an antibacterial agent in the existing blended antibacterial polyurethane are effectively solved. The data show that the antibacterial rate of the obtained macromolecular antibacterial polyurethane memory cotton is up to 99% according to the national standard GB/T20944, and the antibacterial rate is up to 98.5% after 50 times of water washing.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the embodiments described are merely exemplary of the invention, and not of the invention in its entirety. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
In the following examples 1 part by weight represents 1 kg. The following examples relate to the starting components which are all commercially available products.
The polyether polyol I is ethylene oxide propylene oxide copolymerized polyether polyol, wherein the EO content is more than or equal to 50%, the molecular weight is 3500-5000, the functionality is 3-4, the primary hydroxyl end capping is more than or equal to 80%, and the moisture content is less than or equal to 0.05%;
the polyether polyol II is slow rebound polyether, the functionality is 3-4, the molecular weight is 500-1000, and the hydroxyl value is 160-340;
the foam stabilizer is polyether modified organic siloxane L580; the composite amine catalyst is A33 catalyst.
Example 1
The embodiment provides a polymer antibacterial polyurethane memory cotton, which is characterized by comprising the following raw material components:
55 parts by weight of polyguanidine modified isocyanate prepolymer;
65 parts of polyether polyol I;
30 parts of polyether polyol II;
1 part by weight of foam stabilizer;
0.6 part by weight of composite amine catalyst;
2.5 parts by weight of water.
The polyguanidine modified isocyanate prepolymer is prepared by the following method:
(S1) taking polyhexamethylene biguanidine hydrochloride with the molecular formula of (C)8H17N5)nxHCl, n is a natural number between 12 and 16, and the polyhexamethylene biguanide hydrochloride is dissolved in polyether polyol I to obtain a mixture; the addition amount of the polyhexamethylene biguanide hydrochloride accounts for 10% of the mass of the polyether polyol I;
(S2) dropwise adding the mixture obtained in the step (S1) into pure isocyanate under the condition of heating and stirring, wherein the mass ratio of the mixture to the isocyanate is 1:5, continuously reacting for 1h at a constant temperature of 80 ℃ after dropwise adding, and cooling to obtain the polyguanidine modified isocyanate prepolymer.
The preparation method of the macromolecular antibacterial polyurethane memory cotton comprises the following steps:
(1) respectively taking polyether polyol I, polyether polyol II, polyether modified organic siloxane L580, A33 catalyst and water, and fully mixing and stirring uniformly at room temperature to obtain a combined material;
(2) and (2) adding the polyguanidine modified isocyanate prepolymer into the combined material obtained in the step (1), fully and uniformly mixing, stirring at a high speed, pouring into a mould for foaming and molding, and curing to obtain the high-molecular antibacterial polyurethane memory cotton. The antibacterial rate of the obtained macromolecular antibacterial polyurethane memory cotton is more than or equal to 90% according to the national standard GB/T20944, and the antibacterial rate is more than or equal to 90% after washing for 50 times.
Example 2
The embodiment provides a polymer antibacterial polyurethane memory cotton, which is characterized by comprising the following raw material components:
30 parts by weight of polyguanidine modified isocyanate prepolymer;
85 parts of polyether polyol I;
15 parts of polyether polyol II;
2 parts by weight of a foam stabilizer;
0.5 part by weight of composite amine catalyst;
4 parts of water.
The polyguanidine modified isocyanate prepolymer is prepared by the following method:
(S1) taking polyhexamethylene biguanidine hydrochloride with the molecular formula of (C)8H17N5)nxHCl, n is a natural number between 12 and 16, and the polyhexamethylene biguanide hydrochloride is dissolved in polyether polyol I to obtain a mixture; the addition amount of the polyhexamethylene biguanide hydrochloride accounts for 10% of the mass of the polyether polyol I;
(S2) dropwise adding the mixture obtained in the step (S1) into crude isocyanate under the conditions of heating and stirring, wherein the mass ratio of the mixture to the isocyanate is 1:5, continuously reacting for 1h at a constant temperature of 80 ℃ after dropwise adding, and cooling to obtain the polyguanidine modified isocyanate prepolymer.
The preparation method of the macromolecular antibacterial polyurethane memory cotton comprises the following steps:
(1) respectively taking polyether polyol I, polyether polyol II, a foam stabilizer, a composite amine catalyst and water, and fully mixing and stirring uniformly at room temperature to obtain a combined material;
(2) and (2) adding the polyguanidine modified isocyanate prepolymer into the combined material obtained in the step (1), fully and uniformly mixing, stirring at a high speed, pouring into a mold, molding by adopting a molding process, and curing to obtain the high-molecular antibacterial polyurethane memory cotton. The antibacterial rate of the obtained macromolecular antibacterial polyurethane memory cotton is more than or equal to 90% according to the national standard GB/T20944, and the antibacterial rate is more than or equal to 90% after washing for 50 times.
Example 3
The embodiment provides a polymer antibacterial polyurethane memory cotton, which is characterized by comprising the following raw material components:
60 parts by weight of polyguanidine modified isocyanate prepolymer;
55 parts of polyether polyol I;
40 parts of polyether polyol II;
0.5 part by weight of foam stabilizer;
1.5 parts by weight of a composite amine catalyst;
2 parts of water.
The polyguanidine modified isocyanate prepolymer is prepared by the following method:
(S1) taking polyhexamethylene biguanidine hydrochloride with the molecular formula of (C)8H17N5)nxHCl, n is a natural number between 12 and 16, and the polyhexamethylene biguanide hydrochloride is dissolved in polyether polyol I to obtain a mixture; the addition amount of the polyhexamethylene biguanide hydrochloride accounts for 10% of the mass of the polyether polyol I;
(S2) dropwise adding the mixture obtained in the step (S1) into the polyol modified isocyanate under the conditions of heating and stirring, wherein the mass ratio of the mixture to the isocyanate is 1:5, continuously reacting for 1h at a constant temperature of 80 ℃ after dropwise adding, and cooling to obtain the polyguanidine modified isocyanate prepolymer.
The preparation method of the macromolecular antibacterial polyurethane memory cotton comprises the following steps:
(1) respectively taking polyether polyol I, polyether polyol II, a foam stabilizer, a composite amine catalyst and water, and fully mixing and stirring uniformly at room temperature to obtain a combined material;
(2) and (2) adding the polyguanidine modified isocyanate prepolymer into the combined material obtained in the step (1), fully and uniformly mixing, stirring at a high speed, pouring into a mould, molding by adopting a continuous foaming process, and curing to obtain the high-molecular antibacterial polyurethane memory cotton. The antibacterial rate of the obtained macromolecular antibacterial polyurethane memory cotton is more than or equal to 90% according to the national standard GB/T20944, and the antibacterial rate is more than or equal to 90% after washing for 50 times.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.
Claims (10)
1. The macromolecular antibacterial polyurethane memory cotton is characterized by comprising the following raw material components:
30-60 parts of polyguanidine modified isocyanate prepolymer;
55-85 parts of polyether polyol I;
15-40 parts of polyether polyol II;
0.5-2 parts by weight of foam stabilizer;
0.5-1.5 parts by weight of composite amine catalyst;
2-4 parts of water.
2. The macromolecular antibacterial polyurethane memory foam according to claim 1, wherein the polyguanidine modified isocyanate prepolymer is prepared by the following method:
(S1) dissolving polyhexamethylene biguanide hydrochloride in polyether polyol I to obtain a mixture;
(S2) dropwise adding the mixture obtained in the step (S1) into isocyanate under the condition of heating and stirring, continuously reacting for a period of time at constant temperature after dropwise adding, and cooling to obtain the polyguanidine modified isocyanate prepolymer.
3. The polymeric antibacterial polyurethane memory foam according to claim 2, wherein in the step (S1), the molecular formula of the polyhexamethylene biguanide hydrochloride is (C)8H17N5)nxHCl, n is a natural number between 12 and 16, and the addition amount of the polyhexamethylene biguanide hydrochloride accounts for 10 percent of the mass of the polyether polyol I.
4. The antibacterial polyurethane memory foam of claim 1 or 3, wherein the polyether polyol I is ethylene oxide-propylene oxide copolymerized polyether polyol, wherein EO content is greater than or equal to 50%, molecular weight is 3500-5000, functionality is 3-4, primary hydroxyl end capping is greater than or equal to 80%, and moisture content is less than or equal to 0.05%.
5. The polymeric antibacterial polyurethane memory foam according to claim 2, wherein in the step (S2), the mass ratio of the mixture to the isocyanate is 1:5, the heating temperature is 80 ℃, and the dropping time is 1 h;
after the addition was complete, the reaction was continued at 80 ℃ for 1 h.
6. The polymeric antibacterial polyurethane memory foam according to claim 2, wherein in the step (S2), the isocyanate is one or more of pure MDI, crude MDI and polyol modified MDI, and the NCO content of the isocyanate is 25.5-33.6%.
7. The polymeric antibacterial polyurethane memory cotton as claimed in claim 1, wherein the polyether polyol II is slow rebound polyether, with functionality of 3-4, molecular weight of 500-.
8. The antibacterial polyurethane memory foam of claim 1, wherein the foam stabilizer is polyether-modified organosiloxane.
9. The antibacterial polyurethane memory foam of claim 1, wherein the complex amine catalyst is one or more of dimethylethanolamine, bis (dimethylaminoethyl) ether, triethylenediamine, and triethylenediamine;
the composite amine catalyst is a closed delayed catalyst or a reaction catalyst.
10. The preparation method of the high-molecular antibacterial polyurethane memory cotton according to claims 1 to 9, characterized by comprising the following steps:
(1) respectively taking polyether polyol I, polyether polyol II, a foam stabilizer, a composite amine catalyst and water, and fully mixing and stirring uniformly at room temperature to obtain a combined material;
(2) and (2) adding the polyguanidine modified isocyanate prepolymer into the combined material obtained in the step (1), fully and uniformly mixing, and forming and curing to obtain the high-molecular antibacterial polyurethane memory cotton.
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| CN202110525377.9A CN113045726A (en) | 2021-05-12 | 2021-05-12 | High-molecular antibacterial polyurethane memory cotton and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116284968A (en) * | 2023-03-24 | 2023-06-23 | 四川大学华西医院 | Solvent-free preparation of shape memory polyurethane/biomass fiber composite foam and method for regulating and controlling plantar pressure of shape memory polyurethane/biomass fiber composite foam |
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| TW200934534A (en) * | 2007-10-05 | 2009-08-16 | Bayer Innovation Gmbh | Polyurethane foams for wound management |
| CN109134812A (en) * | 2018-07-13 | 2019-01-04 | 汕头大学 | A kind of composite antibacterial polyurethane blocks polymer and its preparation and application |
| CN110305289A (en) * | 2019-07-29 | 2019-10-08 | 福建大方睡眠科技股份有限公司 | A kind of non yellowing polyurethane memory cotton and preparation method thereof |
-
2021
- 2021-05-12 CN CN202110525377.9A patent/CN113045726A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200934534A (en) * | 2007-10-05 | 2009-08-16 | Bayer Innovation Gmbh | Polyurethane foams for wound management |
| CN109134812A (en) * | 2018-07-13 | 2019-01-04 | 汕头大学 | A kind of composite antibacterial polyurethane blocks polymer and its preparation and application |
| CN110305289A (en) * | 2019-07-29 | 2019-10-08 | 福建大方睡眠科技股份有限公司 | A kind of non yellowing polyurethane memory cotton and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116284968A (en) * | 2023-03-24 | 2023-06-23 | 四川大学华西医院 | Solvent-free preparation of shape memory polyurethane/biomass fiber composite foam and method for regulating and controlling plantar pressure of shape memory polyurethane/biomass fiber composite foam |
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Application publication date: 20210629 |