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A kind of preparation method of high molecular weight medicinal polyvinylpyrrolidone

The technology of polyvinylpyrrolidone and vinylpyrrolidone is applied in the fields of medicine, chemical industry and synthetic polymer, and can solve the problems such as difficulty in meeting pharmacopoeia requirements, difficulty in achieving uniform mixing, increase in energy consumption, etc. Guaranteed quality effect

Active Publication Date: 2016-02-17
HUZHOU SHENHUA HIGH POLYMER MATERIAL
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  • Abstract
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Problems solved by technology

[0004] For example, the US patent US4795802 uses activated carbon, ion exchange resin and zeolite to treat the polymer solution to eliminate residual NVP, and the residual NVP after treatment is >10ppm, which is difficult to meet the above pharmacopoeia requirements
Chinese patent 92115179.9 uses ultrafiltration technology to remove residual NVP, which is only suitable for PVP with a K value of 10-45; German patent DE1645642 discloses a method of extracting NVP with an extractant under ultrasonic waves, but it will cause toxic extractants to remain in the polymer
U.S. Patent USP6465592 and Chinese Patent ZL01800010.X use organic peroxides and sulfites as polymerization initiators, and the residual NVP can be reduced to below 10ppm, but the polymerization solution contains 0.25% to 1.0% sulfate ion SO 4 2- and sulfite ion SO 3 2- , does not meet the above-mentioned pharmacopoeia standards, and because it contains the above-mentioned acid radical ions, the resulting product PVP is not completely soluble in organic solvents such as alcohol, which also does not meet the above-mentioned pharmacopoeia standards
Chinese patent ZL01800011.8 is to solve the above-mentioned problem that the above-mentioned Chinese patent ZL01800010.X exists, adopts the acid ion SO 4 2- and SO 3 2- The polymerization solution is removed by anion exchange resin, but this method is not suitable for high molecular weight PVP, such as PVPK90 (K value = 81-96) polymerization solution
Because the viscosity of the 20% concentration polymerization solution of PVPK90 is above 15000mPa.s, regardless of the method of dispersing the anion exchange resin in the polymerization solution or passing the polymerization solution through a fixed bed of anion exchange resin, it is difficult to produce due to the high viscosity of the polymerization solution. To achieve the purpose of uniform mixing, free flow, and easy separation of liquid and solid phases, unless it is highly diluted, which will increase the energy consumption during drying several times
Chinese patent ZL200710105080.7 adopts the method of adding citric acid, lactic acid, malonic acid, etc. to hydrolyze the residual NVP after the polymerization rate reaches more than 99.8%, and then neutralizes it with guanidine carbonate and triethanolamine, so that a large amount of NVP is added to the PVP polymer. Impurities without safety verification also do not meet the requirements of the above Pharmacopoeia

Method used

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  • A kind of preparation method of high molecular weight medicinal polyvinylpyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Put 3400kg of pure water into the reaction kettle equipped with heat exchange coil, nitrogen inlet pipe and stirrer, start the stirrer, introduce nitrogen and heat. After 20 minutes, 800kg of NVP was added, and when the material in the kettle was heated to 70°C, 1.0kg of azobisisobutyronitrile was added to initiate the polymerization reaction. Control material temperature fluctuations not greater than 2°C. After 5 hours, raise the temperature of the material to 75°C, and add 0.4 kg of a composite initiator of azobisisobutyronitrile and tert-butyl hydroperoxide mixed in a ratio of 1:0.3 every 4 hours, and throw in 4 times in total. After the last initiator was added, the reaction was maintained for another 8 hours, and the total polymerization time was 25 hours. The polymerization solution is filtered through a stainless steel mesh filter with a pore size of 1 μm, and then continuously enters a belt-type vacuum dryer, and is dried for 1.0 to 2.5 hours under the conditio...

Embodiment 2

[0021] 3400kg of pure water was dropped into the reactor described in Example 1, stirring was started, nitrogen was introduced and heated, and 800kg of NVP was dropped after 20 minutes. When the material was heated to 60°C, 1.5kg of a composite initiator of azobisisobutyronitrile and azobisisovaleronitrile mixed at a ratio of 1:1 was put in to initiate the polymerization reaction. Control the temperature fluctuation of the material to not exceed 2°C. After 6 hours, adjust the temperature of the material to 70°C. After that, add 0.5 kg of the above-mentioned composite initiator once every 5 hours, and throw 5 times in total. After the last input, the temperature was raised to 75° C., and the reaction was terminated after maintaining for 8 hours. The total polymerization time was 34 hours. After the polymerization solution was vacuum-dried and crushed at low temperature as described in Example 1, the obtained product was tested according to the Pharmacopoeia, and the data are s...

Embodiment 3

[0023] Put 3400kg of pure water into the reactor described in Example 1, start stirring, introduce nitrogen and heat, put in 800kg of NVP after 20 minutes, and when the material is heated to 65°C, put in azodiisocyanurate mixed in a ratio of 1:0.3 The composite initiator 1.2kg of butyronitrile and azobisisovaleronitrile initiates the polymerization reaction. Control the temperature fluctuation of the material not to exceed 2°C, adjust the temperature of the material to 75°C for 6 hours, add 0.4kg of the above-mentioned composite initiator, and then add 0.4kg each time every 4 hours, and throw 5 times in total. After the last input, the temperature was raised to 80° C., and the reaction was terminated after maintaining for 8 hours. The total polymerization time was 34 hours. After the polymerization solution was vacuum-dried and crushed at low temperature as described in Example 1, the obtained product was tested according to the Pharmacopoeia, and the data are shown in Table ...

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Abstract

The invention discloses a preparation method of a medicinal polyvinylpyrrolidone with high molecular weight, which belongs to the fields of medicine chemical industry and synthetic polymer technology. The method concretely the following steps: putting water, N-vinyl pyrrolidone (NVP) and initiator into a reaction vessel in order, stirring and heating, generating a polymerization of NVP, after the reaction ends, filtering the polymer fluid, drying and crushing, and obtaining the finished product. The invention has the beneficial effect that, adsorption and ultrafiltration or the like are not needed for refining the polymer fluid, therefore the energy consumption of drying added for greatly dilution of the high viscosity polymer fluid which is used for improving refining efficiency and yield is avoided, simultaneously a lot of waste water generated in adsorption, ultrafiltration and other refining methods is avoided, thereby saving the waste water treatment process matched thereof. The invention employs continuous low temperature drying and crushing, thereby substantially improving production efficiency and protecting the product quality.

Description

technical field [0001] The present invention relates to a kind of preparation method of polymer, relate in particular to the preparation method of the povidone of composite pharmaceutical specification, more specifically, the present invention relates to the preparation method of high molecular weight, high-purity povidone of composite American, European Pharmacopoeia standard, The invention belongs to the technical field of medicine chemical industry and synthetic polymer. Background technique [0002] PVP is widely used in pharmaceutical production as a pharmaceutical excipient (Povidone, namely Povidone). The pharmacopoeias of various countries, especially the current pharmacopoeias of the United States, Europe, Japan, etc., have quality standards for povidone, especially for the impurities N-vinylpyrrolidone (hereinafter referred to as NVP), 2-pyrrolidone, formic acid, aldehydes, peroxides, There are strict requirements on the content of hydrazine, etc., and no other ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F126/10A61K47/32
Inventor 吴稼祥萧崇宁
Owner HUZHOU SHENHUA HIGH POLYMER MATERIAL
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