CN114085483B - Preparation method of completely biodegradable disposable infusion hose - Google Patents
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- CN114085483B CN114085483B CN202111422620.0A CN202111422620A CN114085483B CN 114085483 B CN114085483 B CN 114085483B CN 202111422620 A CN202111422620 A CN 202111422620A CN 114085483 B CN114085483 B CN 114085483B
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/08—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving unsaturated carbon-to-carbon bonds
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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Abstract
The invention discloses a preparation method of a completely biodegradable disposable infusion hose, which relates to the technical field of medical consumables, and adopts two toughening modification means for polylactic acid, wherein one is to adopt poly (1,1, 1-trimethyl-N-2-propylene propylamine silane) as a monomer to graft and modify the polylactic acid, and the other is to adopt polybutylene succinate to blend and modify the polylactic acid, and the combination of the two toughening modification methods can obviously improve the toughening effect and substantially improve the mechanical property of the polylactic acid; the disposable transfusion hose prepared from the modified polylactic acid has high use safety and the characteristic of complete biodegradation.
Description
The technical field is as follows:
the invention relates to the technical field of medical consumables, in particular to a preparation method of a completely biodegradable disposable infusion hose.
Background art:
a disposable infusion set is a common medical consumable, and a channel between a vein and liquid medicine is established through aseptic treatment and is used for intravenous infusion. Generally, the infusion apparatus is formed by connecting eight parts, namely a vein needle or an injection needle, a needle head protective cap, an infusion hose, a liquid medicine filter, a flow rate regulator, a drip cup, a bottle stopper puncture outfit, an air filter and the like, and a part of the infusion apparatus also comprises an injection piece, a medicine adding port and the like.
The traditional infusion apparatus is mostly made of DEHP plasticized PVC materials, but when the PVC infusion apparatus is clinically used for infusing lipophilic medicaments such as paclitaxel, ciprofloxacin, cefoperazone sodium, fluconazole, metronidazole hydrochloride, cimetidine, fat emulsion and the like, the properties of the medicaments have an enhancement effect on the dissolution of the DEHP, and a plasticizer migrates out and causes harm to a human body along with the entry of liquid medicine into the human body; secondly, due to the poor thermal stability of PVC, a heat stabilizer needs to be added during processing, and the heat stabilizer containing Ca, Zn, Ba and other elements can enter a human body during infusion; furthermore, the PVC resin has a very small amount of vinyl chloride monomer remaining therein, and this compound has been confirmed to be a carcinogenic substance; in addition, the PVC material does not belong to biodegradable plastics, and has the problem of difficult degradation after being discarded, and the defects influence the application of the PVC material in the preparation of disposable infusion sets.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of a completely biodegradable disposable infusion hose, and particularly adopts 1,1, 1-trimethyl-N-2-propylene propylamine silane as a monomer to graft and modify polylactic acid, and adopts polybutylene succinate to blend and modify the polylactic acid, so that the mechanical property of the polylactic acid can be greatly improved, and the biodegradability of the material is ensured.
The technical problem to be solved by the invention is realized by adopting the following technical scheme:
the invention provides a preparation method of a completely biodegradable disposable infusion hose, which comprises the following preparation steps:
(1) uniformly mixing dried polylactic acid, 1,1, 1-trimethyl-N-2-propylene propylamine silane and an initiator in a high-speed mixer to obtain a mixture I;
(2) adding the mixture I obtained in the step (1) into a double-screw extruder, and extruding and granulating to obtain modified polylactic acid I;
(3) uniformly mixing the dried polybutylene succinate and the modified polylactic acid I prepared in the step (2) in a high-speed mixer to obtain a mixture II;
(4) adding the mixture II obtained in the step (3) into a double-screw extruder, and extruding and granulating to obtain modified polylactic acid II;
(5) and (3) adding the modified polylactic acid II prepared in the step (4) into a double-screw extruder, and performing extrusion molding to obtain the disposable infusion hose.
The number average molecular weight of the polylactic acid is 50000-200000g/mol, and the molecular weight distribution is 1.5-5.0.
The mass ratio of the polylactic acid to the 1,1, 1-trimethyl-N-2-propylene propylamine silane is (92-95) to (5-8).
The initiator is an organic peroxide initiator.
The temperature of each section of the double-screw extruder in the step (2) is as follows: the charging section 165-170 ℃, the compression section 180-185 ℃, the metering section 185-190 ℃ and the die head 185-190 ℃; the rotating speed is 100-400 r/min.
The mass ratio of the modified polylactic acid I to the polybutylene succinate is (80-90) to (10-20).
The temperature of each section of the double-screw extruder in the step (4) is as follows: the charging section is 155-160 ℃, the compression section is 170-175 ℃, the metering section is 175-180 ℃, and the die head is 175-180 ℃; the rotating speed is 100-400 r/min.
The temperature of each section of the double-screw extruder in the step (5) is as follows: the charging section is 155-160 ℃, the compression section is 175-180 ℃, the metering section is 185-190 ℃, and the die head is 185-190 ℃; the rotating speed is 100-400 r/min.
The polylactic acid is a biodegradable polymer prepared by chemical synthesis by taking renewable plant resources as raw materials, can be subjected to various molding processing like common polymers, such as extrusion, injection molding, blow molding, cast film forming and the like, and has good biocompatibility and biodegradability. Polylactic acid is high in strength and rigidity, but poor in toughness and impact resistance, and is a hard and brittle material at room temperature, and therefore, it is necessary to modify the toughness of polylactic acid. The blending modification method is an economic polylactic acid toughening modification method, can effectively improve the toughness of polylactic acid, but has the problem of poor compatibility among blending components, so that the mechanical property of a blended system is obviously reduced, and even the biodegradation performance of the material is influenced.
The poly (butylene succinate) is a polymer with good biodegradability and excellent in mechanical property, the poly (butylene succinate) added into a polylactic acid system can toughen and simultaneously retain the original biodegradation characteristic of polylactic acid, but the compatibility of the polylactic acid and the poly (butylene succinate) is poor, and the mechanical property of the blended system cannot achieve an ideal effect.
According to the invention, 1,1, 1-trimethyl-N-2-propylene propylamine silane is adopted to graft and modify polylactic acid, so that on one hand, the polylactic acid can be toughened, on the other hand, the prepared graft modified polylactic acid has good compatibility with polybutylene succinate, and a compatilizer is not required to be additionally added when the polylactic acid is blended and modified by the polybutylene succinate.
Researches find that 1,1, 1-trimethyl-N-2-propylene propylamine silane can replace glycidyl methacrylate and maleic anhydride which are disclosed in the field to have better modification effect on polylactic acid.
The invention also provides another preparation method of the completely biodegradable disposable infusion hose, which comprises the following preparation steps:
(1) uniformly mixing dried polylactic acid, polybutylene succinate, 1, 6-hexanediol diglycidyl ether and hexamethylene diamine in a high-speed mixer to obtain a mixture;
(2) adding the mixture obtained in the step (1) into a double-screw extruder, and extruding and granulating to obtain modified polylactic acid;
(3) adding the modified polylactic acid prepared in the step (2) into a double-screw extruder, and performing extrusion molding to obtain the disposable infusion hose.
The number average molecular weight of the polylactic acid is 50000-200000g/mol, and the molecular weight distribution is 1.5-5.0.
The mass ratio of the polylactic acid to the polybutylene succinate to the 1, 6-hexanediol diglycidyl ether is (80-90) to (10-20) to (1-5), and the use amount of the hexamethylene diamine is based on the condition that all epoxy groups contained in the 1, 6-hexanediol diglycidyl ether are reacted.
The temperature of each section of the double-screw extruder in the step (2) is as follows: the charging section is 155-160 ℃, the compression section is 170-175 ℃, the metering section is 175-180 ℃, and the die head is 175-180 ℃; the rotating speed is 100-400 r/min.
The temperature of each section of the double-screw extruder in the step (3) is as follows: the charging section is 155-160 ℃, the compression section is 175-180 ℃, the metering section is 185-190 ℃, and the die head is 185-190 ℃; the rotating speed is 100-400 r/min.
The invention adopts the polymer of 1, 6-hexanediol diglycidyl ether and hexamethylene diamine (epoxy group and amino group have polycondensation reaction) as the compatilizer, can effectively improve the blending compatibility of polylactic acid and poly butylene succinate, and prevents the blending modification from generating adverse effect on the mechanical property of the system.
The invention has the beneficial effects that:
(1) the invention adopts two toughening modification methods for polylactic acid, one is to adopt poly (1,1, 1-trimethyl-N-2-propylene propylamine silane) as a monomer to graft and modify the polylactic acid, and the other is to adopt polybutylene succinate to blend and modify the polylactic acid, and the combined use of the two toughening modification methods can obviously improve the toughening effect and substantially improve the mechanical property of the polylactic acid.
(2) The disposable infusion hose prepared by the invention has high use safety, does not cause harm to human bodies, has the characteristic of complete biodegradation, and effectively solves the problem of environmental pollution caused by the abandonment of the conventional disposable infusion hose.
The specific implementation mode is as follows:
in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described in the following combined with the specific embodiments.
Polylactic acid was purchased from REVODE110, a bio-material ltd, hai, zhejiang.
Polybutylene succinate is available from basf C1200, germany.
Example 1
(1) Uniformly mixing 95 parts of dried polylactic acid, 5 parts of 1,1, 1-trimethyl-N-2-propylene propylamine silane and 1 part of dicumyl peroxide in a high-speed mixer to obtain a mixture I.
(2) Adding the mixture I obtained in the step (1) into a double-screw extruder, wherein the feeding section is 165 ℃, the compression section is 180 ℃, the metering section is 190 ℃, the die head is 190 ℃, the rotating speed is 300r/min, and extruding and granulating to obtain the modified polylactic acid I.
(3) And (3) uniformly mixing 15 parts of dried polybutylene succinate and 85 parts of modified polylactic acid I prepared in the step (2) in a high-speed mixer to obtain a mixture II.
(4) And (3) adding the mixture II obtained in the step (3) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 170 ℃, the metering section is 175 ℃, the die head is 180 ℃, and the rotating speed is 300r/min, and extruding and granulating to obtain the modified polylactic acid II.
(5) And (5) adding the modified polylactic acid II prepared in the step (4) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 175 ℃, the metering section is 185 ℃, the die head is 185 ℃, the rotating speed is 200r/min, and performing extrusion molding to obtain the disposable infusion hose.
Example 2
(1) And uniformly mixing 92 parts of dried polylactic acid, 8 parts of 1,1, 1-trimethyl-N-2-propylene propylamine silane and 1 part of tert-butyl peroxybenzoate in a high-speed mixer to obtain a mixture I.
(2) Adding the mixture I obtained in the step (1) into a double-screw extruder, wherein the feeding section is 170 ℃, the compression section is 180 ℃, the metering section is 185 ℃, the die head is 190 ℃, and the rotating speed is 200r/min, and extruding and granulating to obtain the modified polylactic acid I.
(3) And (3) uniformly mixing 10 parts of dried polybutylene succinate and 90 parts of modified polylactic acid I prepared in the step (2) in a high-speed mixer to obtain a mixture II.
(4) And (3) adding the mixture II obtained in the step (3) into a double-screw extruder, wherein the feeding section is 155 ℃, the compression section is 170 ℃, the metering section is 175 ℃, the die head is 175 ℃, the rotating speed is 200r/min, and extruding and granulating are carried out to obtain the modified polylactic acid II.
(5) And (3) adding the modified polylactic acid II prepared in the step (4) into a double-screw extruder, wherein the feeding section is 155 ℃, the compression section is 175 ℃, the metering section is 190 ℃, the die head is 190 ℃, the rotating speed is 200r/min, and performing extrusion molding to obtain the disposable infusion hose.
Example 3
(1) And (2) uniformly mixing 93 parts of dried polylactic acid, 7 parts of 1,1, 1-trimethyl-N-2-propylene propylamine silane and 1 part of tert-butyl peroxybenzoate in a high-speed mixer to obtain a mixture I.
(2) Adding the mixture I obtained in the step (1) into a double-screw extruder, wherein the feeding section is 165 ℃, the compression section is 185 ℃, the metering section is 190 ℃, the die head is 190 ℃, the rotating speed is 300r/min, and extruding and granulating to obtain the modified polylactic acid I.
(3) And (3) uniformly mixing 20 parts of dried polybutylene succinate and 80 parts of modified polylactic acid I prepared in the step (2) in a high-speed mixer to obtain a mixture II.
(4) And (3) adding the mixture II obtained in the step (3) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 175 ℃, the metering section is 180 ℃, the die head is 180 ℃, and the rotating speed is 200r/min, and extruding and granulating to obtain the modified polylactic acid II.
(5) And (3) adding the modified polylactic acid II prepared in the step (4) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 175 ℃, the metering section is 185 ℃, the die head is 185 ℃, and the rotating speed is 200r/min, and performing extrusion molding to obtain the disposable infusion hose.
Example 4
(1) Uniformly mixing 80 parts of dried polylactic acid, 20 parts of polybutylene succinate, 5 parts of 1, 6-hexanediol diglycidyl ether and hexamethylene diamine (the amount of hexamethylene diamine is based on that all epoxy groups contained in the 1, 6-hexanediol diglycidyl ether are reacted) in a high-speed mixer to obtain a mixture.
(2) And (2) adding the mixture obtained in the step (1) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 175 ℃, the metering section is 180 ℃, the die head is 180 ℃, and the rotating speed is 200r/min, and extruding and granulating to obtain the modified polylactic acid.
(3) And (3) adding the modified polylactic acid prepared in the step (2) into a double-screw extruder, wherein the feeding section is 155 ℃, the compression section is 175 ℃, the metering section is 185 ℃, the die head is 190 ℃, the rotating speed is 200r/min, and performing extrusion molding to obtain the disposable infusion hose.
Example 5
(1) Uniformly mixing 90 parts of dried polylactic acid, 10 parts of polybutylene succinate, 3 parts of 1, 6-hexanediol diglycidyl ether and hexamethylene diamine (the amount of hexamethylene diamine is based on that all epoxy groups contained in the 1, 6-hexanediol diglycidyl ether are reacted) in a high-speed mixer to obtain a mixture.
(2) And (2) adding the mixture obtained in the step (1) into a double-screw extruder, wherein the feeding section is 155 ℃, the compression section is 170 ℃, the metering section is 175 ℃, the die head is 180 ℃, and the rotating speed is 300r/min, and extruding and granulating to obtain the modified polylactic acid.
(3) Adding the modified polylactic acid prepared in the step (2) into a double-screw extruder, wherein the feeding section is 160 ℃, the compression section is 180 ℃, the metering section is 185 ℃, the die head is 185 ℃, the rotating speed is 200r/min, and performing extrusion molding to obtain the disposable infusion hose.
Comparative example 1
Comparative example 1 differs from example 1 only in that the 1,1, 1-trimethyl-N-2-propenylaminosilane is replaced by an equal amount of glycidyl methacrylate.
Comparative example 2
Comparative example 2 differs from example 1 only in that the 1,1, 1-trimethyl-N-2-propenylaminosilane is replaced by an equal amount of maleic anhydride.
Comparative example 3
Comparative example 3 differs from example 4 only in that the same amount of maleic anhydride-grafted polylactic acid was used instead of hexanediol diglycidyl ether and hexamethylenediamine.
The tensile property is tested according to the standard GB/T1040.1-2018, and the tensile rate is 5 mm/min.
The impact performance is tested according to the standard GB/T1043 + 1993, and a simple beam gapless style impact method is adopted.
The test results are shown in Table 1.
TABLE 1
| Tensile Strength (MPa) | Impact Strength (KJ/m) 2 ) | |
| Example 1 | 39.8 | 24.2 |
| Example 2 | 37.5 | 22.6 |
| Example 3 | 42.7 | 25.3 |
| Example 4 | 31.2 | 16.7 |
| Examples5 | 27.4 | 15.1 |
| Comparative example 1 | 35.6 | 18.5 |
| Comparative example 2 | 32.3 | 17.2 |
| Comparative example 3 | 26.5 | 14.3 |
As can be seen from Table 1, the graft modification of polylactic acid by using 1,1, 1-trimethyl-N-2-propylene propylamino silane can substantially improve the mechanical properties of the prepared material, and the polymer prepared by reacting 1, 6-hexanediol diglycidyl ether and hexamethylenediamine can be used as a compatilizer to achieve the technical effect of improving the mechanical properties of the prepared material.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation method of the completely biodegradable disposable infusion hose is characterized by comprising the following preparation steps:
(1) uniformly mixing dried polylactic acid, 1,1, 1-trimethyl-N-2-propylene propylamine silane and an initiator in a high-speed mixer to obtain a mixture I;
(2) adding the mixture I obtained in the step (1) into a double-screw extruder, and extruding and granulating to obtain modified polylactic acid I;
(3) uniformly mixing the dried polybutylene succinate and the modified polylactic acid I prepared in the step (2) in a high-speed mixer to obtain a mixture II;
(4) adding the mixture II obtained in the step (3) into a double-screw extruder, and extruding and granulating to obtain modified polylactic acid II;
(5) and (5) adding the modified polylactic acid II prepared in the step (4) into a double-screw extruder, and performing extrusion molding to obtain the disposable infusion hose.
2. The method of claim 1, wherein: the number average molecular weight of the polylactic acid is 50000-200000g/mol, and the molecular weight distribution is 1.5-5.0.
3. The production method according to claim 1, characterized in that: the mass ratio of the polylactic acid to the 1,1, 1-trimethyl-N-2-propylene propylamine silane is (93-95) to (5-7).
4. The method of claim 1, wherein: the initiator is an organic peroxide initiator.
5. The method of claim 1, wherein: the temperature of each section of the double-screw extruder in the step (2) is as follows: the charging section 165-170 ℃, the compression section 180-185 ℃, the metering section 185-190 ℃ and the die head 185-190 ℃; the rotating speed is 100-400 r/min.
6. The method of claim 1, wherein: the mass ratio of the modified polylactic acid I to the poly butylene succinate is (80-90) to (10-20).
7. The method of claim 1, wherein: the temperature of each section of the double-screw extruder in the step (4) is as follows: the charging section is 155-160 ℃, the compression section is 170-175 ℃, the metering section is 175-180 ℃, and the die head is 175-180 ℃; the rotating speed is 100-400 r/min.
8. The production method according to claim 1, characterized in that: the temperature of each section of the double-screw extruder in the step (5) is as follows: the charging section is 155-160 ℃, the compression section is 175-180 ℃, the metering section is 185-190 ℃, and the die head is 185-190 ℃; the rotating speed is 100-400 r/min.
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| CN202111422620.0A CN114085483B (en) | 2021-11-26 | 2021-11-26 | Preparation method of completely biodegradable disposable infusion hose |
| PCT/CN2021/133975 WO2023092548A1 (en) | 2021-11-26 | 2021-11-29 | Preparation method for disposable infusion hose capable of being completely biodegraded |
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| CN109096650B (en) * | 2018-08-17 | 2020-12-25 | 江西洪达医疗器械集团有限公司 | Method for preparing remaining needle infusion hose |
| JP6763619B1 (en) * | 2019-05-09 | 2020-09-30 | ヴァス ネットワークス （エイチケー） リミテッドＶａｓｕ Ｎｅｔｗｏｒｋｓ （Ｈｋ） Ｌｔｄ． | How to prepare highly biodegradable materials |
| CN111040400A (en) * | 2019-12-27 | 2020-04-21 | 周锐 | Full-biodegradable sheet and preparation method thereof |
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2021
- 2021-11-26 CN CN202111422620.0A patent/CN114085483B/en active Active
- 2021-11-29 WO PCT/CN2021/133975 patent/WO2023092548A1/en unknown
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| WO2010056421A1 (en) * | 2008-11-13 | 2010-05-20 | Clemson University Research Foundation | Copolymer including polylactic acid, acrylic acid and polyethylene glycol and processes for making the same |
| CN105602211A (en) * | 2014-11-21 | 2016-05-25 | 合肥杰事杰新材料股份有限公司 | Modified nano silica reinforcing and toughening polylactic acid composite material and preparation method thereof |
| CN105623217A (en) * | 2016-02-27 | 2016-06-01 | 江苏金扬子包装科技有限公司 | Polylactic acid bio-based special material for disposable syringe |
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| WO2023092548A1 (en) | 2023-06-01 |
| CN114085483A (en) | 2022-02-25 |
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