CN110699014B - Hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and preparation method thereof - Google Patents
Hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and preparation method thereof Download PDFInfo
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- CN110699014B CN110699014B CN201911116789.6A CN201911116789A CN110699014B CN 110699014 B CN110699014 B CN 110699014B CN 201911116789 A CN201911116789 A CN 201911116789A CN 110699014 B CN110699014 B CN 110699014B
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- sensitive adhesive
- melt pressure
- adhesive matrix
- polyisobutylene
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 30
- 239000012943 hotmelt Substances 0.000 title claims abstract description 30
- 239000011159 matrix material Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 229920002367 Polyisobutene Polymers 0.000 claims abstract description 30
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004927 clay Substances 0.000 claims abstract description 20
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 18
- 239000004945 silicone rubber Substances 0.000 claims abstract description 18
- 239000004014 plasticizer Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 230000008961 swelling Effects 0.000 claims abstract description 4
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 239000004113 Sepiolite Substances 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims description 5
- 229910052900 illite Inorganic materials 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052901 montmorillonite Inorganic materials 0.000 claims description 5
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical compound [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 claims description 5
- 229910052624 sepiolite Inorganic materials 0.000 claims description 5
- 235000019355 sepiolite Nutrition 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 3
- 239000005662 Paraffin oil Substances 0.000 claims description 2
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 claims description 2
- 229910001919 chlorite Inorganic materials 0.000 claims description 2
- 229910052619 chlorite group Inorganic materials 0.000 claims description 2
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052621 halloysite Inorganic materials 0.000 claims description 2
- 230000035699 permeability Effects 0.000 abstract description 5
- 239000002131 composite material Substances 0.000 abstract 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 239000011505 plaster Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 230000007547 defect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000010690 paraffinic oil Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and a preparation method thereof. The medical hot-melt pressure-sensitive adhesive matrix comprises the following components in parts by weight: 65-75 parts of polyisobutylene, 25-35 parts of methyl vinyl silicone rubber, 5-15 parts of plasticizer and 5-10 parts of silicate clay. The preparation method comprises the following steps: firstly, soaking polyisobutylene in a plasticizer until swelling, then melting and blending the swelled polyisobutylene and the methyl vinyl silicone rubber, and then adding silicate clay for blending to obtain the high-performance polyisobutylene/methyl vinyl silicone rubber composite material. The medical hot-melt pressure-sensitive adhesive matrix has a hot-melt pressure-sensitive adhesive matrix similar to a bicontinuous phase structure, and has good hydrophilicity and air permeability.
Description
Technical Field
The invention relates to a hot-melt pressure-sensitive adhesive, in particular to a hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and a preparation method thereof.
Background
The Hot Melt Pressure Sensitive Adhesive (HMPSA) integrates the double characteristics of hot melt and pressure sensitive, is coated in a molten state, can be bonded by applying small finger pressure after being cooled and solidified, and changes the physical state by changing the temperature. Compared with the traditional solvent-based pressure-sensitive adhesive, the hot-melt pressure-sensitive adhesive has the advantages of simple process, safety and environmental protection.
From the prior art, most of hot melt pressure sensitive adhesives are prepared by taking one or more polymer materials as a substrate and then assisting with various auxiliaries, the hot melt pressure sensitive adhesives are rarely further improved on the structure of the substrate, and especially in the application of medical plasters, the hot melt pressure sensitive adhesives still have some obvious defects, such as: the medical plaster has insufficient hydrophilicity and air permeability, which causes the limitation of the types and the components of the medicines which can be loaded by the medical plaster, and the poor air permeability and the poor perspiration effect under the state that the plaster is attached to the skin.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix comprises the following components in parts by weight:
65-75 parts of polyisobutylene, 25-35 parts of methyl vinyl silicone rubber, 5-15 parts of plasticizer and 5-10 parts of silicate clay.
In the above technical scheme, the weight parts of the components are preferably as follows: 68-72 parts of polyisobutylene, 28-38 parts of methyl vinyl silicone rubber, 8-12 parts of a plasticizer and 5-10 parts of silicate clay; more preferably: 70 parts of polyisobutylene, 30 parts of methyl vinyl silicone rubber, 10 parts of plasticizer and 5-10 parts of silicate clay.
In the above technical solution, the polyisobutylene is high molecular weight polyisobutylene, and preferably polyisobutylene N50.
In the above technical solution, the plasticizer is selected as in the prior art, and preferably naphthenic oil and/or paraffinic oil.
In the above technical solution, the silicate clay is selected from the same as the prior art, and is preferably one or a combination of two or more selected from kaolin, montmorillonite, illite, chlorite, halloysite and sepiolite. The silicate clay is subjected to acidification and impurity removal treatment before use, and specifically, the silicate clay is placed in dilute acid, soaked for 1-3 hours under a heating condition (usually 50-80 ℃), taken out and washed to be neutral by water. The dilute acid can be dilute hydrochloric acid or dilute sulfuric acid, and the molar concentration is usually 1-3 mol/L.
The invention also provides a preparation method of the hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix, which is characterized by comprising the following steps:
1) weighing the components according to the formula for later use;
2) soaking polyisobutylene in plasticizer until swelling;
3) and melting and blending the swelled polyisobutylene and the methyl vinyl silicone rubber, and then adding silicate clay for blending to obtain the hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix.
In step 3) of the preparation method, the melt blending is usually performed in a rubber internal mixer, the temperature and time during internal mixing are the same as those in the prior art, preferably, the swollen polyisobutylene and the methyl vinyl silicone rubber are mixed at the temperature of 160-180 ℃ (the rotating speed is 50-80r/min) for 30-50min, and the swollen polyisobutylene and the methyl vinyl silicone rubber are mixed at the temperature of 160-180 ℃ (the rotating speed is 50-80r/min) for 30-50min after the silicate clay is added.
Compared with the prior art, the polyisobutylene is placed in the plasticizer to swell, and then is blended with the methyl vinyl silicone rubber and the silicate clay to disperse the silicate clay in the matrix to obtain the hot-melt pressure-sensitive adhesive matrix with the structure similar to a bicontinuous phase, and the obtained matrix has good hydrophilicity and air permeability.
Drawings
FIG. 1 is an electron microscope scanning image of the hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix prepared in example 1 of the present invention.
Detailed Description
The present invention will be better understood from the following detailed description of specific examples, which should not be construed as limiting the scope of the present invention.
Example 1
(1) The formula is as follows:
70 parts of polyisobutylene (polyisobutylene N50), 30 parts of methyl vinyl silicone rubber, 10 parts of plasticizer (paraffin oil) and 10 parts of silicate clay (sepiolite); wherein, the sepiolite is subjected to the following impurity removal treatment in advance: putting sepiolite into hydrochloric acid with the concentration of 1mol/L, stirring and soaking for 2h at 70 ℃, taking out, washing with water to be neutral, and drying.
(2) The preparation method comprises the following steps:
weighing each component according to a formula for later use;
soaking polyisobutylene in plasticizer until swelling;
placing the swelled polyisobutylene and the methyl vinyl silicone rubber in a rubber internal mixer, and mixing at 180 ℃ at a rotating speed of 50r/min for 20 min; then adding silicate clay, and mixing at 180 ℃ at a rotating speed of 20r/min for 40min to obtain the hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix. As shown in the figure of an electron microscope scanning image of the medical hot-melt pressure-sensitive adhesive matrix, as can be seen from figure 1, the methyl vinyl silicone rubber and the polyisobutylene N50 form a bicontinuous phase structure, and a phase interface provides an air permeability channel, so that the air tightness of the matrix is weakened.
At room temperature, 3g of the medical hot-melt pressure-sensitive adhesive matrix and the pure adhesive matrix (polyisobutylene N50) prepared in the embodiment are respectively taken as samples, pressed into a film with the thickness of about 1mm at 120 ℃ by a flat vulcanizing instrument, sealed on a conical bottle opening of 50ml, filled with a certain amount of absolute ethyl alcohol, and the mass of the absolute ethyl alcohol is weighed after 24 hours. The mass of the matrix was recorded at 0h and 21h, respectively, and the results are shown in Table 1 below.
Table 1:
Q＝(M0-M1)/πr2
wherein Q represents a gas transmission amount per unit area, g/cm2(ii) a M0 represents the mass of absolute ethanol, g, ventilated for 24 hours; m1 represents the mass of initial absolute ethanol, g; pi r2Indicates the area of the conical opening in cm2Wherein r is in cm).
The gas transmission of absolute ethyl alcohol through a 1mm substrate film was calculated according to the above formula, and the results were as follows:
q (pure gum base) ═ 0.002g/cm2；
Q (example 1) 0.024g/cm2。
1g of the medical hot-melt pressure-sensitive adhesive matrix and the pure adhesive matrix (polyisobutylene N50) prepared in the example were respectively used as samples at room temperature, and the samples were placed in distilled water and weighed for 24 hours. The mass of the matrix was recorded at 0h and 21h, respectively, and the results are shown in Table 2 below.
Table 2:
w％＝(M1-M0)/M0
wherein w% represents water absorption, M1 represents the mass of the sample after 24 hours of water absorption, g; m0 denotes the initial mass of the sample, g.
The water absorption was calculated according to the above formula and the results were as follows:
w% (pure gum base) is 0.9%.
w% (example 1) 19%.
Example 2
(1) The formula is as follows:
75 parts of polyisobutylene (polyisobutylene N50), 25 parts of methyl vinyl silicone rubber, 15 parts of plasticizer (naphthenic oil) and 5 parts of silicate clay (illite); wherein, illite is subjected to the following impurity removal treatment in advance: putting illite into hydrochloric acid with the concentration of 2mol/L, stirring and soaking for 2 hours at the temperature of 60 ℃, taking out, washing with water to be neutral, and drying.
(2) The preparation method comprises the following steps:
the same as in example 1.
Example 3
(1) The formula is as follows:
65 parts of polyisobutylene (polyisobutylene N50), 35 parts of methyl vinyl silicone rubber, 10 parts of plasticizer (comprising wax oil and naphthenic oil in a weight ratio of 1: 1) and 8 parts of silicate clay (comprising montmorillonite and kaolin in a weight ratio of 1: 1); wherein, the montmorillonite and the kaolin are subjected to the following impurity removal treatment in advance: taking montmorillonite and kaolin, respectively stirring and soaking with 1mol/L sulfuric acid at 60 deg.C for 2h, taking out, washing with water to neutrality, and drying.
(2) The preparation method comprises the following steps:
the same as in example 1.
Claims (5)
1. A hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix comprises the following components in parts by weight:
polyisobutylene N5065-75 parts, methyl vinyl silicone rubber 25-35 parts, plasticizer 5-15 parts, and silicate clay 5-10 parts.
2. The hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix according to claim 1, wherein: the weight parts of each component are as follows:
polyisobutylene N5070 parts, methyl vinyl silicone rubber 30 parts, plasticizer 10 parts and silicate clay 5-10 parts.
3. The hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix according to claim 1 or 2, wherein: the plasticizer is naphthenic oil and/or paraffin oil.
4. The hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix according to claim 1 or 2, wherein: the silicate clay is one or more of kaolin, montmorillonite, illite, chlorite, halloysite and sepiolite.
5. The preparation method of the hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix as claimed in claim 1, wherein the preparation method comprises the following steps:
1) weighing the components according to the formula for later use;
2) soaking polyisobutylene N50 in the plasticizer until swelling;
3) and melting and blending the swelled polyisobutylene N50 and the methyl vinyl silicone rubber, and then adding silicate clay for blending to obtain the hydrophilic breathable medical hot-melt pressure-sensitive adhesive matrix.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911116789.6A CN110699014B (en) | 2019-11-15 | 2019-11-15 | Hydrophilic and breathable medical hot-melt pressure-sensitive adhesive matrix and preparation method thereof |
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| CN110699014B true CN110699014B (en) | 2021-06-18 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174309A (en) * | 2011-01-13 | 2011-09-07 | 深圳市森日有机硅材料有限公司 | Solvent-free organic silicon pressure-sensitive adhesive and preparation method thereof |
| CN107629735A (en) * | 2016-07-19 | 2018-01-26 | 上海暖友实业有限公司 | Special hot-fusible pressure-sensitive adhesive of medical plaster and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4557305B2 (en) * | 2003-06-19 | 2010-10-06 | 日東電工株式会社 | Rubber adhesive composition and adhesive sheet thereof |
| CN102153868A (en) * | 2011-01-13 | 2011-08-17 | 滁州天成有机硅高分子材料有限公司 | Production formula of silicon rubber gross rubber |
| CN104910856A (en) * | 2015-05-29 | 2015-09-16 | 成都亨通光通信有限公司 | Optical fiber surface coating adhesive |
| CN106433135A (en) * | 2016-09-08 | 2017-02-22 | 黄品超 | Curable rubber composition and curable rubber |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102174309A (en) * | 2011-01-13 | 2011-09-07 | 深圳市森日有机硅材料有限公司 | Solvent-free organic silicon pressure-sensitive adhesive and preparation method thereof |
| CN107629735A (en) * | 2016-07-19 | 2018-01-26 | 上海暖友实业有限公司 | Special hot-fusible pressure-sensitive adhesive of medical plaster and preparation method thereof |
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