CN115779156A

CN115779156A - Deiodination viscose composition and operation film thereof

Info

Publication number: CN115779156A
Application number: CN202211628705.9A
Authority: CN
Inventors: 娄非非; 鲁建国
Original assignee: Zhende Medical Co Ltd
Current assignee: Zhende Medical Co Ltd
Priority date: 2022-12-16
Filing date: 2022-12-16
Publication date: 2023-03-14

Abstract

The invention discloses a deiodination viscose composition and an operation film thereof, which comprise a prepolymer, an initiator, a cross-linking agent, a solvent, acetic acid and a stabilizer; acetic acid accounts for 15-25% of the mass of the ingredients of the composition and is used as a main deiodination component. The content of acetic acid is improved by adding the stabilizer, the volatile smell is greatly reduced, and the high-efficiency deiodination is realized. The surgical film coated with the backing film has good peel strength, and simultaneously improves the problem of reduced skin stickiness of the surgical site after iodophor sterilization.

Description

Deiodination viscose composition and operation film thereof

Technical Field

The invention relates to a disposable consumable in the field of medical care, in particular to an operation film for closing an operation wound, and specifically relates to a deiodination viscose composition and an operation film thereof.

Background

Currently, iodine wound disinfection liquid used clinically mainly comprises anidine, povidone iodine and the like, the operation part and the periphery of a patient need to be disinfected in a large range before an operation, iodophor solution is generally used for treatment, and an operation film is attached to the solution after the solution is dried to perform the operation. The iodophor has a lasting bactericidal effect, the iodophor solution has a surface activity effect, the iodophor used for wiping the dry surgical site before the operation causes the adhesive property between the surgical membrane and the skin to be reduced, and if the iodophor is used for deiodination during the operation, the treatment effect is not good, the treatment time is long, and the workload of medical staff is increased.

The operation membrane provides a better solution for creating a good sterile environment for an operation position and inhibiting skin bacteria. The iodine is not absorbed to cause 'channel' and pathogenic bacteria can continuously breed and move on the surface of the skin and around the operation incision, so that the Infection (SSI) of the operation Site can be caused.

Disclosure of Invention

The purpose of the invention is as follows: an object of the present invention is to provide a sustained-release type deiodination adhesive composition which takes acetic acid as a main deiodination component and effectively prevents the acetic acid from volatilizing; the invention also aims to provide a method for preparing the deiodination operating membrane by coating the deiodination adhesive composition; it is still another object of the present invention to provide a deiodinated surgical membrane obtained by the aforementioned preparation method.

The technical scheme is as follows: in order to achieve the aim, the deiodination viscose composition comprises a prepolymer, an initiator, a cross-linking agent, a solvent, acetic acid and a stabilizer; the acetic acid accounts for 15-25% of the mass of the ingredients of the composition, the stabilizing agent accounts for 10-15% of the mass of the ingredients of the composition, and the stabilizing agent is selected from any one or more of 8-hydroxyquinoline, phosphoric acid, sodium pyrophosphate, sodium silicate, potassium dihydrogen phosphate and sodium hexametaphosphate.

The prepolymer of the present invention may be selected from an acrylic prepolymer or a polyurethane prepolymer. Wherein, the acrylic prepolymer includes but is not limited to any one or more of methyl acrylate, ethyl acrylate, fluorinated ethyl acrylate, isooctyl acrylate, butyl acrylate and lauryl acrylate; the polyurethane prepolymer is selected from any one or combination of more of diisocyanate, triisocyanate, polyether and polyester polyol. The combination of methyl acrylate, ethyl acrylate, isooctyl acrylate and fluoro ethyl acrylate is preferably adopted, and the obtained polymer has good thermal stability, acid and alkali corrosion resistance, good water repellent effect and dirt resistance. The mass ratio of methyl acrylate to ethyl acrylate is preferably 1:1, the mass ratio of fluoro ethyl acrylate to methyl acrylate is preferably 1 (1.5-2), isooctyl acrylate accounts for 50-90wt% of the total amount of the prepolymer, and the addition amount of the prepolymer accounts for 30-45wt% of the total composition.

Further, the initiator is selected from any one or more of azodiisobutyronitrile, benzoyl peroxide, di-tert-butyl peroxide and lauroyl peroxide. Preference is given to using azobisisobutyronitrile in amounts of from 0.1 to 3% by weight. In practice, the monomer conversion can be increased by batchwise addition of the initiator.

Further, the crosslinking agent is selected from any one or more of divinylbenzene, N-methylolacrylamide, hydroxypropyl methacrylate and diacetone acrylamide. Divinylbenzene is preferably used, which has good cohesion as a crosslinking agent and has no adhesive residue. The amount added is preferably 0.5 to 5% by weight.

The invention creatively adds the stabilizing agent to reduce the volatility of the irritant acid and delay the release. The stabilizer is selected from any one or more of 8-hydroxyquinoline, phosphoric acid, sodium pyrophosphate, sodium silicate, potassium dihydrogen phosphate and sodium hexametaphosphate, and 8-hydroxyquinoline and/or phosphoric acid are preferably adopted.

Optionally, essence can be further added to relieve pungent sour taste, and the fruit flavor with sour fragrance, such as lemon flavor, is particularly suitable for selection.

As a further optimization of the invention, the composition also comprises 0.1-10wt% of oxalic acid. Preferably, the oxalic acid is added in an amount of 3 to 8wt%. In general, the adding amount of acetic acid is not less than 15 percent, the adding amount of oxalic acid is not less than 3 percent, and the whole system has better compatibility and can provide better deiodination performance. But also produces a strong pungent acid taste and affects the use experience. This problem is well alleviated by the addition of stabilizers.

As a further optimization of the invention, the composition also comprises 0.01-1wt% of vitamin C. Preferably, the vitamin C is added in an amount of 0.05-2wt%. The addition of oxalic acid and vitamin C is beneficial to improving the deiodination effect of the product, and skin allergy or desquamation which may exist in case of too high addition amount is avoided. Those skilled in the art can selectively add the compounds within the proper range under the inventive principle of the present application, and the compounds are within the scope of the present invention.

As a further optimization of the invention, the composition also comprises 0.1-3wt% of sodium thiosulfate, and the sodium thiosulfate is preferably added in an amount of 0.5-2wt%. Sodium thiosulfate can be added into the deiodinated component to prevent skin allergy or desquamation.

Further, the solvent comprises any one or combination of ethanol, isopropanol, and ethyl acetate. Wherein, ethyl acetate is mainly used as a solvent in a polymerization system, and ethanol is a main solvent of the deiodination component.

The invention provides a preparation method of a deiodination surgical membrane, which comprises the following steps:

(1) Stirring a part of prepolymer in a water bath at constant temperature under the protection of nitrogen, and adding a part of initiator when obvious reflux occurs;

(2) Adding the rest of prepolymer and the other part of initiator;

(3) Adding the rest of initiator, cross-linking agent, ethanol and acetic acid under constant temperature, and stirring to obtain deiodinated viscose;

(4) Coating the deiodination viscose glue on the surface of a backing film in the thickness of 1-500 mu m, firstly drying for the first time, then attaching release paper, and then drying and curing for the second time to obtain a finished product.

The formula of the prepolymer added in the step (1) is as described above, and the addition amount of the prepolymer accounts for 30-70% of the whole mass. The remaining 30% -60% of the prepolymer is used in step (2). This is intended to be a stepwise polymerization, which makes the polymerization reaction more complete. Similarly, the initiator is added in batches in the step (1), the step (2) and the step (3) to improve the monomer conversion rate. The backing film used in the step (4) can be selected from any one of materials including, but not limited to, PE, PU and TPU. The coating thickness is 20 + -5 um, preferably 20 + -3 um, and the coating is cured in an oven at 60-90 deg.C for 6-18 hr to obtain the final product.

Based on the deiodination adhesive composition and the deiodination operation membrane prepared by the method, according to the standard of YY/0852-2011 on disposable sterile operation membranes, the normal-temperature stripping force of 180 degrees is measured to be 10-14N/25mm, skin damage does not occur during stripping, the holding adhesive displacement is 0mm, the adhesion is not easy to fall off, the higher the initial adhesive 32# value is, the adhesion cannot be influenced by iodophor after being pasted. After being adhered to the surface of the skin for 2 minutes after being sterilized by the iodophor, the content of iodide ions can be reduced to below 7ppm, the deiodination effect is directly achieved, and the problem of reduction of the skin viscosity of the operation part after being sterilized by the iodophor is solved. According to the invention, the addition of the stabilizer is increased to over 15%, and the product has no volatile odor.

Detailed Description

The present invention is further illustrated by the following specific examples. The percentages in the examples are percentages by mass, unless otherwise specified.

Example 1

The embodiment provides a deiodination viscose composition, which comprises the following components in percentage by mass:

wherein the prepolymer consists of 5.5 percent of methyl acrylate, 9.5 percent of ethyl acrylate, 64 percent of isooctyl acrylate and 21 percent of fluorinated ethyl acrylate.

The preparation method of 1000g of the deiodination viscose composition by using the formula comprises the following steps:

(1) 50% ethyl acetate, 50% methyl acrylate, 50% ethyl acrylate, 50% isooctyl acrylate, 50% ethyl fluoroacrylate were added to a flask, and after a condenser tube and a separatory funnel were fitted and the other tube ports were sealed, nitrogen protection was turned on. Then starting an electric stirring and constant-temperature water bath kettle for heating, controlling the rotation speed to be uniform, keeping the temperature of the solvent in the flask uniform and maintaining the temperature at 90 +/-1 ℃, and adding 30% of initiator when obvious reflux occurs;

(2) Uniformly mixing 50% of ethyl acetate, 50% of methyl acrylate, 50% of ethyl acrylate, 50% of isooctyl acrylate and 50% of ethyl fluoroacrylate, adding the mixture into a separating funnel connected to a flask, mixing the inner walls of the used beaker before washing with ethyl acetate after the mixture is added, then adding a washing solvent into the separating funnel, and adding 40% of an initiator;

(3) And after the heat preservation is carried out for 2 hours, adding 30% of initiator, continuing to carry out the heat preservation for 3 hours, adding ethanol, acetic acid, sodium thiosulfate, oxalic acid and vitamin C, stirring, and discharging after stirring for 2 hours.

(4) Weighing 26g of the synthesized deiodination viscose composition, starting coating, ensuring the coating thickness to be 20 +/-1 um, putting the mixture into an oven at 80 ℃ for baking for 5min, attaching common release paper, putting the mixture into the oven at 70 ℃ for curing for 12h, and obtaining the deiodination surgical membrane.

Example 2

1000g of the deiodinated viscose composition was prepared as above for the formulation using the same method as in example 1. And weighing 26g of the synthesized deiodination viscose composition, starting to coat a sample, ensuring the coating thickness to be 20 +/-1 mu m, baking for 5min in an oven at 80 ℃, attaching common release paper, and curing for 12h in the oven at 70 ℃ to obtain the deiodination surgical membrane.

Example 3

1000g of the deiodinated viscose composition was prepared as above for the formulation using the same method as in example 1. Then weighing 26g of the synthesized deiodination viscose composition, starting coating, ensuring the coating thickness to be 20 +/-1 um, putting the mixture into an oven at 80 ℃ for baking for 5min, attaching common release paper, putting the mixture into the oven at 70 ℃ for curing for 12h, and obtaining the deiodination surgical membrane.

Example 4

wherein the prepolymer consists of 10.5 percent of methyl acrylate, 39.5 percent of ethyl acrylate, 29 percent of isooctyl acrylate and 21 percent of fluorinated ethyl acrylate.

(1) Adding all ethyl acetate, methyl acrylate, ethyl acrylate, fluoro ethyl acrylate, ethanol, acetic acid, sodium thiosulfate, oxalic acid, vitamin C and sodium silicate in the formula into a flask at one time, installing a condenser tube and a separating funnel, sealing other tube openings, and then opening nitrogen protection. And then starting an electric stirring and constant-temperature water bath kettle for heating, controlling the rotation speed to be uniform, keeping the temperature of the solvent in the flask uniform and maintaining the temperature at 90 +/-1 ℃, adding all the initiators when obvious reflux occurs, stirring for 2 hours, and then discharging.

(2) Weighing 26g of the synthesized deiodination viscose composition, starting coating, ensuring the coating thickness to be 20 +/-1 um, putting the mixture into an oven at 80 ℃ for baking for 5min, attaching common release paper, putting the mixture into the oven at 70 ℃ for curing for 12h, and obtaining the deiodination surgical membrane.

Test example 1 adhesion test

30 subjects were selected from 30 specimens.

Simulation test: the ordinary operation film and the operation film with the deiodination effect obtained in the above embodiment are used for trial pasting for 2 hours, and the pasting effect is observed. Simulating an operating room scene, taking a sample, sticking the sample to the left side and the right side of the abdomen (one side is a common operating film, the other side is a deiodination operating film), using a cotton swab to dip povidone iodine solution to wipe a part to be pasted, wherein the wiping area is larger than the product area, and sticking a product after the iodine solution is dried. The product can not stretched when pasting, pastes and levels no fold, and the operator can not touch dressing and paste the face, and the test result is shown in table 1:

TABLE 1 adhesion test

As can be seen from Table 1, the deiodination surgical films provided in examples 1-3 have good adhesion, wherein the best effect is obtained in example 1, the adhesion and prepolymer content are in a certain positive correlation, and the effect of example 4 is greatly different due to the prepolymer formula and preparation method.

Test example 2 Peel Strength test

Based on the peel strength test of YY/0852-2011 "Disposable sterile surgical Membrane", the sample roll (sheet) should be left at 23 + -1 deg.C and 50 + -5% humidity for 24h or more. Before the test specimen, the test panel was cleaned (wiped with ethyl acetate, no blue light) and then could not be touched with a finger. And (5) airing for at least 10 minutes.

Three test specimens, each having a width (24. + -. 0.5) mm and a length of about 30cm, were cut at different portions of the deiodinated surgical membrane and the general surgical membrane of examples 1 to 4. When the sample width is less than 24mm, the test is performed with the actual width of the sample and noted in the test results. When the tape width is more than 24mm, a predetermined sample is cut out.

Three test specimens 25mm wide and about 30cm long were cut out in different sections. When the sample width is less than 25mm, the test is performed with the actual width of the sample and noted in the test results. When the width of the adhesive tape is more than 25mm, a predetermined sample is cut out.

The cut sample is attached to a 180 DEG test plate (5 cm multiplied by 12 cm) (the sample position is centered), and the sample is placed on an adhesive tape press roller (operated according to the operation instruction of the adhesive tape press roller) or a manual press roller to roll the sample back and forth three times at the speed of 600mm/min (the bonding part of the sample and the test plate is not allowed to have air bubbles). The rolled samples were left to stand at 23 ℃ 1 ℃ and 50% + -5% humidity for about 20 minutes before testing (GB/T2792-1998).

The tail end of the sample is pasted with release paper, the non-smooth surface is pasted on the sample, then one end of the sample is folded by 180 degrees, one end of the steel plate is clamped in a clamp of an electronic stripping machine, and the free end of the adhesive tape is clamped in the other clamp (the stripping surface is consistent with the force line of the testing machine).

And selecting a 'stripping' key on the stripping machine, wherein the stripping indicator lamp displays red, then pressing a 'test' button, starting stripping by the testing machine at the speed of 300mm/min +/-10 mm/min until a stop key is pressed at a position 2cm away from the tail end of the sample, and recording data (in a unit of N) displayed by a display screen, namely the 180-degree stripping value. And pressing a return key to automatically return the instrument.

From test data, the peel force at the normal temperature of 180 ℃ is 10-14N/25mm, skin damage can not occur during peeling, the holding viscosity displacement is 0mm, the adhesive is not easy to fall off, the higher the initial viscosity 32# value is, and the viscosity is not influenced by iodophor after the adhesive is pasted.

Test example 3

Based on the addition of 19% acetic acid in example 1, the rest samples with different acetic acid addition contents are provided, weighed and placed in a 60 ℃ oven, and taken out after being dried for 1 hour, so that the deiodination rate is determined to rise along with the rise of the acetic acid content, and tends to be gentle when reaching about 90%, and the addition amount of 19% acetic acid is optimal in consideration of volatility and irritation.

Acetic acid%	The deiodination rate%
		0	0
4	5％
		9	50％
14	70％
		19	90％
24	91％

The above description is only of the preferred embodiments of the present invention, and it should be noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.

Claims

1. A deiodinated adhesive composition characterized by: comprises prepolymer, initiator, cross-linking agent, solvent, acetic acid and stabilizer; the acetic acid accounts for 15-25% of the mass of the ingredients of the composition, the stabilizing agent accounts for 10-15% of the mass of the ingredients of the composition, and the stabilizing agent is selected from any one or more of 8-hydroxyquinoline, phosphoric acid, sodium pyrophosphate, sodium silicate, potassium dihydrogen phosphate and sodium hexametaphosphate.

2. The deiodinated adhesive composition of claim 1, wherein: the prepolymer is methyl acrylate, ethyl acrylate, isooctyl acrylate and fluoro ethyl acrylate.

3. A deiodinated adhesive composition as defined in claim 2, wherein: the crosslinking agent is divinylbenzene.

4. A deiodinated adhesive composition as defined in claim 3, wherein: the composition further comprises 0.1-10% oxalic acid.

5. A deiodinated adhesive composition as defined in claim 3, wherein: the composition further comprises 0.01-1% of vitamin C.

6. A deiodinated adhesive composition as defined in claim 3, wherein: the composition further comprises 0.01-3% sodium thiosulfate.

7. A deiodinated adhesive composition as defined in claim 3, wherein: the initiator is selected from any one of azodiisobutyronitrile, benzoyl peroxide, di-tert-butyl peroxide and lauroyl peroxide.

8. A preparation method of a deiodination surgical membrane is characterized by comprising the following steps: the deiodinated adhesive composition of claim 1 is prepared by the following steps:

(2) Adding the rest of prepolymer and the other part of initiator;

9. The method of claim 8, wherein the step of preparing a surgical membrane comprises: the prepolymer added in the step (1) accounts for 30-70% of the total addition amount of the prepolymer.

10. The deiodinated surgical film obtained by the method of claim 9.