CN110790962A - Preparation method of nitrocellulose film - Google Patents
Preparation method of nitrocellulose film Download PDFInfo
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- CN110790962A CN110790962A CN201911215404.1A CN201911215404A CN110790962A CN 110790962 A CN110790962 A CN 110790962A CN 201911215404 A CN201911215404 A CN 201911215404A CN 110790962 A CN110790962 A CN 110790962A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/14—Chemical modification with acids, their salts or anhydrides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/08—Cellulose derivatives
- C08J2301/16—Esters of inorganic acids
- C08J2301/18—Cellulose nitrate
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Abstract
The invention discloses a preparation method of a nitrocellulose film, which comprises the following specific steps: preparing a membrane preparation solution, coating, drying and post-processing, performing hydrophilic treatment and performing sterile treatment to obtain the nitrocellulose membrane. The preparation method of the nitrocellulose membrane enables the digestive cellulose membrane to have better hydrophilicity, the concentration of the added surfactant is very low, but the surfactant has great influence on final membrane formation, the content of the surfactant is high, the size of the membrane forming aperture can be controlled, the membrane preparation solution is assisted with a controlled production process environment, an ideal membrane forming structure can be obtained, the aperture of the membrane can be ideally controlled, and the nitrocellulose membrane can be finally applied to products for rapid diagnosis through proper post-treatment, hydrophilic treatment and sterile treatment.
Description
Technical Field
The invention belongs to the technical field of nitrocellulose membrane preparation methods, and particularly relates to a preparation method of a nitrocellulose membrane.
Background
Nitrocellulose, which is a product of the esterification reaction of cellulose and nitric acid, has good film-forming properties, and is one of the earliest high-molecular polymers used for preparing films in the world. In 1908 Bechhold immersed filter paper coated with nitrocellulose solution in glacial acetic acid produced a first artificial membrane whose permeability was adjusted by varying the ratio of nitrocellulose to glacial acetic acid. Nitrocellulose was also used in the study by Zsigmondy, which in 1918 used a membrane made from nitrocellulose to separate large molecules from small particles in aqueous solutions.
In recent years, due to the high molecular characteristics of nitrocellulose itself, applications thereof are gradually shifted from filtration and separation to bioanalysis with higher added value, and the application is mainly benefited from the nonspecific adsorption capacity of nitrocellulose to substances such as proteins. On the other hand, in the application of rapid diagnosis products, the membrane is required to have hydrophilicity, and due to the self hydrophobicity of the nitrocellulose, the requirement is put forward on the post-treatment of the membrane. At present, the film in China basically depends on import.
On the other hand, the application of rapid diagnostic products requires that the membrane has hydrophilicity, and the hydrophobicity of the nitrocellulose itself also demands the hydrophilic post-treatment of the membrane. Different hydrophilic treatments can have a dramatic effect on the performance of the membrane, thereby altering the product performance of the diagnostic product.
Disclosure of Invention
The invention aims to provide a preparation method of a nitrocellulose film, which solves the problem of poor hydrophilicity of the nitrocellulose film, and makes the product application more reliable by aseptic processing.
The technical scheme adopted by the invention is as follows: preparation method of nitrocellulose film
Step 1: dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution;
step 2: coating the film-forming solution on a continuously running stainless steel belt or plastic supporting substrate, wherein the thickness of the coated wet film is 150-;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 5-15% of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 0.5-20 minutes to obtain a membrane;
and 5: after post-treatment, the film is dried at the temperature of 25-75 ℃;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 0.5-2h at the temperature of 40-65 ℃ to obtain the nitrocellulose membrane.
The present invention is also characterized in that,
the nitrocellulose membrane added raw materials in the step 1 comprise the following components in percentage by weight: 5-30% of nitrocellulose, 18-30% of acetone, 5-12% of water, 30-65% of cosolvent and 0.01-2% of surfactant, wherein the sum of the mass percentages of the above materials is 100%.
In the step 2, the plastic supporting base material is a PET base material, and the thickness of the plastic supporting base material is 20-500 mu m.
In the step 3, the temperature of the drying tunnel is 15-40 ℃, and the relative humidity is 40-99%; and/or the temperature of the drying tunnel is 20-30 ℃, and the relative humidity is 65-90%; the air exhaust amount in the drying tunnel is controlled to be 0.01-8% of the concentration of the solvent steam.
And 4, the post-treatment solution in the step 4 is one or more mixed aqueous solutions of sulfate or sulfonate anionic surfactants.
The surfactant in the step 1 is one or a mixture of more of an anionic surfactant and glycerol.
Step 7 the hydrophilic treatment solution is an alkylpolyglycoside surfactant solution.
The invention has the beneficial effects that:
the preparation method of the nitrocellulose membrane enables the digestive cellulose membrane to have better hydrophilicity, the concentration of the added surfactant is very low, but the surfactant has great influence on final membrane formation, the content of the surfactant is high, the size of the membrane forming aperture can be controlled, the membrane preparation solution is assisted with a controlled production process environment, an ideal membrane forming structure can be obtained, the aperture of the membrane can be ideally controlled, and the nitrocellulose membrane can be finally applied to products for rapid diagnosis through proper post-treatment, hydrophilic treatment and sterile treatment.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
Step 1: weighing the following materials in percentage by mass: 5% of nitrocellulose, 30% of acetone, 12% of water, 52.99% of cosolvent and 0.01-2% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 20 μm, wherein the thickness of the coated wet film is 150 μm;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the temperature of the drying tunnel is 15 ℃, and the relative humidity is 40; controlling the concentration of solvent vapor to be 0.01% by the exhaust air quantity in the drying tunnel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 5 percent of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 0.5 minute, so as to obtain a membrane;
the post-treatment solution is a mixed aqueous solution of sulfate salt and sulfonate anionic surfactant.
And 5: drying the film at 25 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 0.5h at the temperature of 40 ℃ to obtain the nitrocellulose membrane.
Example 2
Step 1: weighing the following materials in percentage by mass: 25% of nitrocellulose, 18% of acetone, 5% of water, 50% of cosolvent and 2% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 500 μm, wherein the thickness of the coated wet film is 850 μm;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the temperature of the drying tunnel is 40 ℃, and the relative humidity is 99 percent; controlling the concentration of solvent vapor to be 8% by the exhaust air quantity in the drying channel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 15% of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 20 minutes to obtain a membrane;
the post-treatment solution is one or more mixed aqueous solutions of sulfate or sulfonate anionic surfactants.
And 5: drying the film at 75 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 0.5-2h at the temperature of 65 ℃ to obtain the nitrocellulose membrane.
Example 3
Step 1: weighing the following materials in percentage by mass: 10% of nitrocellulose, 19% of acetone, 5% of water, 65% of cosolvent and 1% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 200 μm, wherein the thickness of the coated wet film is 200 μm;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the temperature of the drying tunnel is 30 ℃, and the relative humidity is 60%; controlling the concentration of solvent vapor to be 5% by the exhaust air quantity in the drying tunnel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 10 percent of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 10 minutes, and soaking the membrane-making liquid for 5 minutes to obtain a membrane;
the post-treatment solution is one or more mixed aqueous solutions of sulfate or sulfonate anionic surfactants.
And 5: drying the film at 50 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 1h at the temperature of 50 ℃ to obtain the nitrocellulose membrane.
Example 4
Step 1: weighing the following materials in percentage by mass: 30% of nitrocellulose, 30% of acetone, 9% of water, 30% of cosolvent and 1% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 20-500 μm, wherein the thickness of the coated wet film is 400 μm;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the drying tunnel temperature is 20 ℃, and the relative humidity is 65%; controlling the concentration of solvent vapor to be 2% by the exhaust air quantity in the drying tunnel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 6 percent of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 5 minutes to obtain a membrane;
the post-treatment solution was a sulfate salt.
And 5: drying the film at 60 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 1h at the temperature of 55 ℃ to obtain the nitrocellulose membrane.
Example 5
Step 1: weighing the following materials in percentage by mass: 20% of nitrocellulose, 20% of acetone, 8% of water, 50% of cosolvent and 2% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 300 μm, wherein the thickness of the coated wet film is 700 μm;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the temperature of the drying tunnel is 30 ℃, and the relative humidity is 90 percent; controlling the concentration of solvent vapor to be 8% by the exhaust air quantity in the drying channel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 5 percent of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 0.55 minute and 0.5 minute to obtain a membrane;
the post-treatment solution is a sulfonate anionic surfactant.
And 5: drying the film at 40 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 2 hours at the temperature of 40 ℃ to obtain the nitrocellulose membrane.
Example 6
Step 1: weighing the following materials in percentage by mass: 20% of nitrocellulose, 20% of acetone, 8% of water, 50% of cosolvent and 2% of surfactant;
dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution, wherein the surfactant is one or a mixture of anionic surfactant and glycerol;
step 2: coating the film-forming solution on a continuously running stainless steel belt or a PET substrate with the thickness of 100 mu m, wherein the thickness of the coated wet film is 600 mu m;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
the temperature of the drying tunnel is 25 ℃, and the relative humidity is 80%; controlling the concentration of solvent vapor to be 7% by the exhaust air quantity in the drying tunnel;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 15% of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 20 minutes and 10 minutes to obtain a membrane;
the post-treatment solution is a mixed aqueous solution of sulfate salt and sulfonate anionic surfactant.
And 5: drying the film at 70 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution, wherein the hydrophilic treatment solution is an alkyl polyglycoside surfactant solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 0.5h at the temperature of 55 ℃ to obtain the nitrocellulose membrane.
According to the method, the digestive cellulose membrane has better hydrophilicity, the concentration of the added surfactant is very low, but the added surfactant has great influence on final membrane formation, the content of the surfactant is high, and the size of the membrane forming aperture can be controlled.
Claims (7)
1. A method for preparing a nitrocellulose membrane is characterized in that,
step 1: dissolving nitrocellulose in acetone, and then adding a cosolvent, water and a surfactant; mixing and stirring uniformly, and filtering to obtain a membrane preparation solution;
step 2: coating the film-forming solution on a continuously running stainless steel belt or plastic supporting substrate, wherein the thickness of the coated wet film is 150-;
and step 3: immediately conveying the stainless steel strip or plastic support base material coated with the film-making liquid to a drying tunnel for controlling temperature, humidity and air inlet and outlet quantity to dry;
and 4, step 4: when the acetone content in the membrane-making liquid is reduced to 5-15% of the initial content, soaking the membrane-making liquid in water for cleaning and dedusting, and then continuously soaking the membrane-making liquid in a post-treatment solution for 0.5-20 minutes to obtain a membrane;
and 5: the film is dried at the temperature of 25-75 ℃ after post-treatment;
step 6: putting the dried film into a hydrophilic treatment solution for continuous soaking treatment or spraying the film by using the hydrophilic treatment solution;
and 7: and (3) performing sterile treatment on the dried film, namely performing low-heat radiation sterilization treatment for 0.5-2h at the temperature of 40-65 ℃ to obtain the nitrocellulose membrane.
2. The method for preparing the nitrocellulose membrane of claim 1, wherein the nitrocellulose membrane added with raw materials in step 1 comprises the following components in percentage by weight: 5-30% of nitrocellulose, 18-30% of acetone, 5-12% of water, 30-65% of cosolvent and 0.01-2% of surfactant, wherein the sum of the mass percentages of the above materials is 100%.
3. The method for preparing nitrocellulose membrane of claim 1, wherein the plastic support substrate in step 2 is a PET substrate having a thickness of 20 to 500 μm.
4. The method for preparing the nitrocellulose membrane of claim 1, wherein the temperature of the drying tunnel in step 3 is 15-40 ℃, and the relative humidity is 40-99%; and/or the temperature of the drying tunnel is 20-30 ℃, and the relative humidity is 65-90%; the air exhaust amount in the drying tunnel is controlled to be 0.01-8% of the concentration of the solvent steam.
5. The method for preparing nitrocellulose membrane of claim 1, wherein the post-treatment solution in step 4 is one or more mixed aqueous solutions of sulfate or sulfonate anionic surfactants.
6. The method for preparing nitrocellulose membrane of claim 1, wherein the surfactant in step 1 is one or more of anionic surfactant and glycerol.
7. The method according to claim 1, wherein the hydrophilic treatment solution in step 7 is an alkylpolyglycoside surfactant solution.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112114132A (en) * | 2020-08-28 | 2020-12-22 | 瑞捷生物科技江苏有限公司 | Carrier fixed with nitrocellulose membrane, preparation method and application thereof |
| WO2022069470A1 (en) * | 2020-09-30 | 2022-04-07 | Merck Patent Gmbh | Nitrocellulose papers and methods of production and use |
| CN115678110A (en) * | 2021-07-29 | 2023-02-03 | 南京理工大学 | Blend film containing nitrocellulose and plasticizer and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819710A (en) * | 2014-03-04 | 2014-05-28 | 苏州奥特福环境科技有限公司 | Method for preparing hydrophilic nitrated cellulose film |
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2019
- 2019-12-02 CN CN201911215404.1A patent/CN110790962A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103819710A (en) * | 2014-03-04 | 2014-05-28 | 苏州奥特福环境科技有限公司 | Method for preparing hydrophilic nitrated cellulose film |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112114132A (en) * | 2020-08-28 | 2020-12-22 | 瑞捷生物科技江苏有限公司 | Carrier fixed with nitrocellulose membrane, preparation method and application thereof |
| WO2022069470A1 (en) * | 2020-09-30 | 2022-04-07 | Merck Patent Gmbh | Nitrocellulose papers and methods of production and use |
| CN115678110A (en) * | 2021-07-29 | 2023-02-03 | 南京理工大学 | Blend film containing nitrocellulose and plasticizer and preparation method thereof |
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