CN111961152A - Polyacrylic resin emulsion as enteric medicine coating material and its prepn - Google Patents
Polyacrylic resin emulsion as enteric medicine coating material and its prepn Download PDFInfo
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- CN111961152A CN111961152A CN202010870242.1A CN202010870242A CN111961152A CN 111961152 A CN111961152 A CN 111961152A CN 202010870242 A CN202010870242 A CN 202010870242A CN 111961152 A CN111961152 A CN 111961152A
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- enteric
- coating material
- polyacrylic resin
- resin emulsion
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/32—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds, e.g. carbomers, poly(meth)acrylates, or polyvinyl pyrrolidone
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/26—Emulsion polymerisation with the aid of emulsifying agents anionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/04—Azo-compounds
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epidemiology (AREA)
- Pharmacology & Pharmacy (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention discloses an enteric drug coating material polyacrylic resin emulsion, which is prepared from the following raw materials in parts by weight: 50-80 parts of methacrylic acid; 1-45 parts of ethyl acrylate; 1-45 parts of butyl acrylate; 0-5 parts of sodium dodecyl sulfate; polysorbate-805-10; 1-8 parts of azobisisobutyronitrile; 350-400 parts of purified water. The invention also discloses a preparation method of the latex. The starting point of the dissolution of the coating material is PH4.5, the pH unit of the enteric coating area extends to the weak acid area, and the pH is increased from the original pH5.5 → 10.0 to the pH4.5 → 10.0, so that the enteric coating material can be used as an auxiliary material of a medicament for treating gastrohelcosis and duodenal diseases; can also be used for coating enteric-coated medicines; it has the characteristics of fast dissolution and higher release rate; the application range is wide.
Description
Technical Field
The invention relates to the technical field of pharmaceutic adjuvants, in particular to polyacrylic resin latex as an enteric drug coating material; the invention also relates to a preparation method of the polyacrylic resin emulsion of the enteric drug coating material.
Background
The enteric coating materials used in China at present are divided into two types according to solvent media:
1) alcohol soluble type, wherein polyacrylic resin II and III, the alcohol soluble type uses ethanol as solvent, has high cost, is inflammable and explosive, has three wastes, and tends to be eliminated at present in China.
2) The aqueous medium, wherein the polyacrylic resin I (methacrylic acid-butyl acrylate copolymer aqueous dispersion) and the methacrylic acid-ethyl acrylate copolymer aqueous dispersion both take water as the medium, the coating cost is low, the product quality is good, the production is safe, and three wastes are avoided, so the coating is the main material for enteric coating at present in China. Therefore, the research on the novel aqueous medium enteric-coated medicament coating material has important significance.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a novel polyacrylic resin emulsion as an enteric drug coating material, the coating material has a low dissolution starting point, and an enteric region extends to a weak acid region by one PH unit, so that the problem of limitation of some release parts at present can be solved.
The invention also aims to provide a preparation method of the polyacrylic resin latex solution, which can be used for industrial production.
The technical problem to be solved by the present invention is achieved by the following technical means. The invention provides an enteric drug coating material polyacrylic resin latex (L30D-45), which is characterized in that the enteric drug coating material polyacrylic resin latex is prepared from the following raw materials in parts by weight:
50-80 parts of methacrylic acid;
1-45 parts of ethyl acrylate;
1-45 parts of butyl acrylate;
0-5 parts of sodium dodecyl sulfate;
polysorbate-805-10;
1-8 parts of azobisisobutyronitrile;
350-400 parts of purified water.
When the sodium dodecyl sulfate is contained in the technical scheme, the weight ratio of the sodium dodecyl sulfate is 0.1-5.
In the polyacrylic resin emulsion as the enteric drug coating material in the technical scheme, the weight ratio of the raw materials is preferably as follows:
66.7 parts of methacrylic acid;
16.6 parts of ethyl acrylate;
16.6 parts of butyl acrylate;
sodium dodecyl sulfate 0.7;
polysorbate-802.3;
azobisisobutyronitrile 1.2;
purified water 230.
The technical problem to be solved by the invention can be further realized by the following technical scheme, and the invention also provides a preparation method of the enteric-coated drug coating material polyacrylic resin emulsion, which is characterized by comprising the following steps:
(1) putting raw materials of purified water, sodium dodecyl sulfate and polysorbate-80 into a reaction tank according to the weight ratio, adding azodiisobutyronitrile, stirring and heating to 75-80 ℃ for later use;
(2) mixing methacrylic acid, ethyl acrylate and/or butyl acrylate, dropwise adding the mixture into a reaction tank under the stirring condition for 3-5 hours, heating to 90-97 ℃ after dropwise adding, maintaining the reaction for 0.5-2.0 hours, and naturally cooling to room temperature to obtain the product.
In the step (1), azobisisobutyronitrile is added as an initiator, and then preferably heated to 75 ℃ with stirring. In the step (2), the time taken for dropping the mixture into the reaction tank is preferably 5 hours.
Compared with the prior art, the invention has the following advantages:
the polyacrylic resin emulsion of the enteric drug coating material has high acid value, can be dissolved in weak acid PH4.5 medium, and can be used as an auxiliary material of a drug for treating gastric pylorus and duodenal diseases; can also be used for coating enteric-coated medicines; it has the characteristics of fast dissolution and higher release rate; the application range is wider.
The coating material can push the dissolution starting point of the existing enteric coating from PH5.5 to PH4.5, the enteric coating area extends a PH unit to the weak acid area, and the pH is increased from the original PH5.5 → 10.0 to PH4.5 → 10.0, so that the coating material can clinically solve the international problems at present, such as the application to the diseases of pylorus and duodenum of the stomach, and the like, and provides a good choice for the medicines which have the puncture to the stomach but have to be released at the parts of pylorus, duodenum, and the like of the stomach.
The polyacrylic resin emulsion of the enteric drug coating material prepared by the method is a copolymer, the average molecular weight of the copolymer is 20 ten thousand, and the ratio of free carbonyl groups to ester groups is about 2: 1, the acid value is 400-430, the pH value of the latex is 1-3, and the anionic copolymer accounts for 28-31% of the total weight of the polyacrylic resin latex. The emulsifier is preferably sodium dodecyl sulfate and polysorbate-80; initiator azobisisobutyronitrile. The particle diameter of the polymerized anionic copolymer contained in the latex is less than 1um, and the polymerized anionic copolymer is insoluble in the latex environment (pH 1-3) and shows Brownian motion, so that the latex has a milky appearance, is stable to stand at room temperature, and is non-toxic and harmless.
Detailed description of the invention
The following further describes particular embodiments of the present invention in order to facilitate a more complete understanding of the present invention by those skilled in the art, and does not constitute a limitation to the rights thereto.
Embodiment 1, a polyacrylic resin latex solution (L30D-45) enteric material, which is prepared from the following raw materials in parts by weight:
80 parts of methacrylic acid;
ethyl acrylate 20;
butyl acrylate 10;
sodium dodecyl sulfate 1.0;
polysorbate-802.5;
azobisisobutyronitrile 2.0;
purified water 260;
can be prepared by conventional polymerization reaction process.
Example 2. An enteric material of polyacrylic resin latex solution (L30D-45) is prepared from the following raw materials in parts by weight:
66.7 parts of methacrylic acid;
16.6 parts of ethyl acrylate;
16.6 parts of butyl acrylate;
sodium dodecyl sulfate 0.7;
polysorbate-802.3;
azobisisobutyronitrile 1.2;
purified water 230;
the preparation method comprises the following steps:
(1) according to the weight ratio, 20% of purified water, sodium dodecyl sulfate and polysorbate-80 are taken, added with azobisisobutyronitrile for pre-emulsification, then put into a reactor containing 80% of purified water, gradually dispersed, stirred and heated to 75 ℃ for later use;
(2) mixing methacrylic acid, ethyl acrylate and/or butyl acrylate, dropwise adding into a reaction tank under stirring for 5 hours, heating to 93 ℃ after dropwise adding, maintaining reaction for 1.0 hour, and naturally cooling to room temperature to obtain the product.
Example 3. An enteric drug coating material of polyacrylic resin latex solution is prepared from the following raw materials in parts by weight:
methacrylic acid 90;
30 parts of ethyl acrylate;
butyl acrylate 15;
0.5 of ammonium persulfate;
sodium dodecyl sulfate 0.6;
polysorbate-801.7;
purified water 280;
the preparation method comprises the following steps:
(1) putting raw materials of purified water, ammonium persulfate, sodium dodecyl sulfate and polysorbate-80 into a reaction tank according to the weight ratio, adding azodiisobutyronitrile for pre-emulsification, stirring and heating to 80 ℃,
(2) mixing methacrylic acid, ethyl acrylate and butyl acrylate, dripping the mixture into a reaction tank under the stirring condition, keeping the temperature for 60 minutes after dripping, heating to 95 ℃, keeping the reaction for 1.0 hour, and naturally cooling to room temperature to obtain the acrylic acid modified acrylic acid.
The polyacrylic resin latex is detected according to the content required by Chinese pharmacopoeia, and the quality indexes are as follows:
1) the characteristics are as follows: milky low viscosity suspension;
2) acid value: 400-430
3) Intrinsic viscosity: 3-10MPSa
4）PH：1-3
5) Residual monomer: less than 0.01 percent
6) The total solid is 30 percent
Effective group (-COOH) content: more than 65 percent.
Claims (5)
1. An enteric-coated drug coating material polyacrylic resin latex is characterized in that: the traditional Chinese medicine is prepared from the following raw materials in parts by weight:
50-80 parts of methacrylic acid;
1-45 parts of ethyl acrylate;
1-45 parts of butyl acrylate;
0-5 parts of sodium dodecyl sulfate;
polysorbate-805-10;
1-8 parts of azobisisobutyronitrile;
350-400 parts of purified water.
2. The enteric-coated drug coating material polyacrylic resin latex solution of claim 1, wherein: the weight ratio of each raw material is as follows:
66.7 parts of methacrylic acid;
16.6 parts of ethyl acrylate;
16.6 parts of butyl acrylate;
sodium dodecyl sulfate 0.7;
polysorbate-802.3;
azobisisobutyronitrile 1.2;
purified water 230.
3. The preparation method of the polyacrylic resin emulsion as the enteric drug coating material of claim 1 or 2, comprising the following steps:
(1) putting raw materials of purified water, sodium dodecyl sulfate and polysorbate-80 into a reaction tank according to the weight ratio, adding azodiisobutyronitrile, stirring and heating to 75-80 ℃ for later use;
(2) mixing methacrylic acid, ethyl acrylate and butyl acrylate, dropwise adding the mixture into a reaction tank under the stirring condition for 3-5 hours, heating to 90-97 ℃ after dropwise adding, maintaining the reaction for 0.5-2.0 hours, and naturally cooling to room temperature to obtain the product.
4. The preparation method of the polyacrylic resin emulsion as the enteric-coated drug coating material of claim 3, wherein the polyacrylic resin emulsion comprises: in the step (1), the mixture is stirred and heated to 75 ℃.
5. The preparation method of the polyacrylic resin emulsion as the enteric-coated drug coating material of claim 3, wherein the polyacrylic resin emulsion comprises: the dropping time in the step (2) was 5 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010870242.1A CN111961152A (en) | 2020-08-26 | 2020-08-26 | Polyacrylic resin emulsion as enteric medicine coating material and its prepn |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010870242.1A CN111961152A (en) | 2020-08-26 | 2020-08-26 | Polyacrylic resin emulsion as enteric medicine coating material and its prepn |
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| Publication Number | Publication Date |
|---|---|
| CN111961152A true CN111961152A (en) | 2020-11-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010870242.1A Pending CN111961152A (en) | 2020-08-26 | 2020-08-26 | Polyacrylic resin emulsion as enteric medicine coating material and its prepn |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921361A (en) * | 2009-06-13 | 2010-12-22 | 孙小冬 | Polyacrylic resin latex for enteric medicine coating material and preparation method thereof |
| CN102382231A (en) * | 2011-09-07 | 2012-03-21 | 张绍国 | Polyacrylic resin I and preparation method thereof |
| CN102432737A (en) * | 2011-09-07 | 2012-05-02 | 张绍国 | Controlled-release enteric acrylic resin latex and preparation method thereof |
| CN105833281A (en) * | 2016-05-18 | 2016-08-10 | 张绍国 | Aqueous enteric film coating premixed agent and preparation method thereof |
-
2020
- 2020-08-26 CN CN202010870242.1A patent/CN111961152A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921361A (en) * | 2009-06-13 | 2010-12-22 | 孙小冬 | Polyacrylic resin latex for enteric medicine coating material and preparation method thereof |
| CN102382231A (en) * | 2011-09-07 | 2012-03-21 | 张绍国 | Polyacrylic resin I and preparation method thereof |
| CN102432737A (en) * | 2011-09-07 | 2012-05-02 | 张绍国 | Controlled-release enteric acrylic resin latex and preparation method thereof |
| CN105833281A (en) * | 2016-05-18 | 2016-08-10 | 张绍国 | Aqueous enteric film coating premixed agent and preparation method thereof |
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Application publication date: 20201120 |