CN115093498B - Preparation method of PVP (polyvinyl pyrrolidone) with low residual monomer and low chromaticity - Google Patents
Preparation method of PVP (polyvinyl pyrrolidone) with low residual monomer and low chromaticity Download PDFInfo
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- CN115093498B CN115093498B CN202210717421.0A CN202210717421A CN115093498B CN 115093498 B CN115093498 B CN 115093498B CN 202210717421 A CN202210717421 A CN 202210717421A CN 115093498 B CN115093498 B CN 115093498B
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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
- C08F126/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen
- C08F126/06—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen by a heterocyclic ring containing nitrogen
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Abstract
The invention provides a preparation method of PVP with low residual monomer and low chromaticity, which relates to the technical field of water-soluble polymers, and is mainly applied to the preparation of PVP with K value smaller than 60, and mainly comprises the following steps: under the protection of nitrogen, pure water, NVP, an initiator and an acid-base modifier are used as reaction liquid for high-temperature polymerization reaction; the pH value interlocking control device monitors the pH value environment of the polymerization liquid on line in real time, ensures that the pH value of the reaction environment is continuously controlled between 7 and 9, greatly improves the polymerization efficiency, ensures that the reaction can be completed in a short time, thereby obviously reducing the high-temperature reaction time and finally obtaining PVP with low residual monomer and low chromaticity.
Description
Technical Field
The invention relates to the technical field of water-soluble polymers, in particular to a preparation method of PVP with low residual monomer and low chromaticity, which is mainly applied to the preparation of PVP with K value less than 60,
background
PVP, collectively referred to as polyvinylpyrrolidone, is a linear polymer of varying degrees of polymerization prepared from N-vinylpyrrolidone (NVP) monomers by homopolymerization. Commercial PVP is graded according to average molecular weight, and different K values respectively represent corresponding PVP average molecular weight ranges, mainly including K15, K25, K30, K45, K60, K90 and the like. PVP has excellent hydrophilicity, film forming property, physiological activity and other performances, and is widely applied to the high and new technical fields of pharmaceutical auxiliary materials, daily chemicals, cosmetics, foods, biomedical materials and the like.
In PVP production, a general and economical method is to use aqueous solution polymerization, hydrogen peroxide is used as an initiator, ammonia water is used as a pH value regulator, in the industrial production process, certain high-temperature conditions are usually required to be ensured in order to achieve the aim of low residual monomers, but the high-temperature time is too long to cause the increase of polymer chromaticity, so that cosmetic grade indexes cannot be achieved, the high-temperature time is insufficient, the residual monomers are higher, and the medical grade and food grade indexes cannot be met, so that the control of the high-temperature time is particularly important.
In the prior art, in order to reduce residual NVP monomer in the polymer, a polymer material post-treatment process, such as activated carbon adsorption, solvent extraction or ultrafiltration, radiation and other modes, are mostly adopted, and the method has good residual removal single effect, but has complex equipment and higher production cost and energy consumption; in the prior art, in order to avoid polymer discoloration caused by overheat of temperature, a method for accurately controlling the reaction temperature by controlling the vacuum degree in a reaction kettle by using a vacuum controller is proposed, and the product produced by the method has the advantages of stable quality, complex process control process and high cost.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a preparation method of PVP with low residual monomer and low chromaticity, which mainly uses a DCS interlocking control device to accurately control the pH value environment of polymerization, thereby effectively improving the polymerization efficiency, shortening the polymerization time, ensuring the completion of the polymerization reaction in a short time, and solving the problems that the existing technology cannot effectively consider both the residual monomer and chromaticity index of the polymer, and the technology is more complex and the cost is higher.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the preparation method of PVP with low residual monomer and low chromaticity is applied to the preparation of PVP with K value smaller than 60, and adopts a pH value interlocking control device, and the pH value of the reaction liquid is monitored on line in real time through a DCS distributed control system, so that the pH value of a polymerization environment is ensured to be continuously controlled between 7 and 9; the method specifically comprises the following steps:
s1, carrying out polymerization reaction at 50-90 ℃ under the protection of nitrogen, taking pure water as a solvent, and adding a certain amount of NVP monomer, hydrogen peroxide and ammonia water;
s2, adding hydrogen peroxide after the reaction is carried out for 60-120 min, and adding hydrogen peroxide every 30-60 min for 2-6 times;
s3, after the total continuous reaction is carried out for 180-300 min, the PVP with low residual monomer and low chromaticity is prepared.
Preferably, the preparation method ensures that the pH value of the polymerization environment is continuously controlled between 8 and 8.5.
Preferably, the preparation method maintains the reaction temperature at 80-90 ℃.
Preferably, in step S1, pure water is added for the first time, wherein the pure water is nvp=55 to 135:45, and hydrogen peroxide is added for the first time, and the NVP monomer is added for the first time, wherein the pure water is added for the first time, and the pure water is added for the first time.
Preferably, pure water: NVP monomer=68 to 84:45 by weight.
Preferably, in step S2, the additional hydrogen peroxide is NVP monomer=10 to 15:1000 by weight.
Preferably, in step S2, the number of times of adding hydrogen peroxide is 3 to 4.
Preferably, in step S2, when the pH value of the polymerization environment is about to deviate from the preset range, the pH value of the polymerization solution is precisely controlled by starting the analysis control valve through the pH value interlocking control device.
(III) beneficial effects
The invention provides a preparation method of PVP with low residual monomer and low chromaticity, which is mainly applied to the preparation of PVP with K value smaller than 60, and the pH of the reaction environment is controlled in real time through a DCS distributed control system, so that the polymerization efficiency is greatly improved, the reaction can be completed in a short time, the high-temperature reaction time is obviously reduced, and finally the PVP with low residual monomer and low chromaticity is obtained.
Compared with the prior art, the method has the following beneficial effects:
(1) The synthesized PVP product has more excellent product quality, the residual monomer is less than or equal to 10ppm, the chroma Hazen is less than or equal to 30 (10% aqueous solution)), and the product meets the indexes of medicine grade, food grade and cosmetic grade.
(2) Compared with the methods of over-active carbon adsorption, reaction kettle vacuum degree control and the like with complex equipment or process control process and high production cost and energy consumption, the method is simpler to operate, more intelligent and saves energy consumption and cost.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is evident that the drawings in the following description are only some embodiments of the present invention and that other drawings may be obtained from these drawings without inventive effort for a person of ordinary skill in the art.
FIG. 1 is a schematic diagram of a preparation method of PVP with low residual monomer and low chromaticity according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of an interlocking control device for ph value according to an embodiment of the present invention.
Wherein, AV: analysis control valve (pH value), AIC: analysis indicates adjustment (PH), TIC: temperature display adjustment, TV: temperature regulating valve, PL: measuring point liquid level, SC: steam condensate, LS: low pressure steam.
Detailed Description
The embodiment of the application solves the problem that the existing technology cannot effectively meet the requirements of polymer residual monomers and chromaticity indexes by providing the preparation method of the PVP with low residual monomers and low chromaticity. The above technical solution will be described in detail below with reference to the accompanying drawings of the specification and several examples and comparative examples.
As shown in fig. 1, the embodiment of the invention provides a preparation method of low-residual-monomer low-chromaticity PVP, which is applied to the preparation of PVP with a K value smaller than 60, and adopts a pH value interlocking control device shown in fig. 2, and the pH value of a reaction solution is monitored on line in real time through a DCS distributed control system, so that the pH value of a polymerization environment is ensured to be continuously controlled between 7 and 9; the method specifically comprises the following steps:
s1, carrying out polymerization reaction at 50-90 ℃ under the protection of nitrogen, taking pure water as a solvent, and adding a certain amount of NVP monomer, hydrogen peroxide and ammonia water;
s2, adding hydrogen peroxide after the reaction is carried out for 60-120 min, and adding hydrogen peroxide every 30-60 min for 2-6 times;
s3, after the total continuous reaction is carried out for 180-300 min, the PVP with low residual monomer and low chromaticity is prepared.
In one embodiment, the preparation method ensures that the pH of the polymerization environment is continuously controlled between 8 and 8.5.
In one embodiment, the preparation process maintains the reaction temperature at 80-90 ℃.
In an embodiment, in step S1, pure water is added for the first time, nvp=55 to 135:45, and hydrogen peroxide is added for the first time, NVP monomer is added for the first time, and NVP monomer is added for the first time, 20 to 28:1000.
In one embodiment, pure water: NVP monomer=68 to 84:45 by weight.
In one embodiment, in step S2, the additional hydrogen peroxide is NVP monomer=10 to 15:1000 by weight.
In one embodiment, in step S2, the hydrogen peroxide is added 3 to 4 times.
In one embodiment, in step S2, when the pH value of the polymerization environment is about to deviate from the preset range, the pH value of the polymerization solution is precisely controlled by starting the analysis control valve through the pH value interlocking control device.
Example 1:
s1, carrying out polymerization under the protection of nitrogen, taking pure water as a solvent, adding 68 parts by weight of NVP monomer and 45 parts by weight of NVP monomer; the pH value is monitored on line in real time by a DCS distributed control system by adopting a pH value interlocking control device, the pH value of the reaction environment is controlled to be 8-8.5, and when the temperature is raised to 50 ℃,35% hydrogen peroxide (35% hydrogen peroxide: NVP monomer=28:1000 by weight) is added;
s2, supplementing hydrogen peroxide (35% hydrogen peroxide: monomer=15:1000 by weight) after the reaction is carried out for 120min, maintaining the reaction temperature between 80 and 90 ℃, and supplementing hydrogen peroxide (35% hydrogen peroxide: monomer=15:1000 by weight) every 60min, wherein the total supplementing is 3 times; during the period, a pH value interlocking control device is adopted, the pH value is monitored on line in real time through a DCS distributed control system, and the pH value of the reaction environment is controlled to be 8-8.5;
s3, after the total duration reaction time is 300min, the reaction is finished, and the PVP with low residual monomer and low chromaticity is prepared.
Samples were taken and the examined polymeric product PVP had a K value of 29.61, residual order of 1.5ppm and Hazen color of 28.6.
Example 2:
s1, carrying out polymerization under the protection of nitrogen, taking pure water as a solvent, adding 84 parts by weight of NVP monomer, and adding 45 parts by weight of NVP monomer; the pH value is monitored on line in real time by a DCS distributed control system by adopting a pH value interlocking control device, the pH value of the reaction environment is controlled to be 8-8.5, and when the temperature is raised to 50 ℃,35% hydrogen peroxide (35% hydrogen peroxide: NVP monomer=20:1000 by weight) is added;
s2, after the reaction is carried out for 60min, adding hydrogen peroxide once (35% hydrogen peroxide by weight: monomer=10:1000), maintaining the reaction temperature at 80-90 ℃, and adding hydrogen peroxide once every 30min later (35% hydrogen peroxide by weight: monomer=10:1000), wherein the total adding time is 4 times; during the period, a pH value interlocking control device is adopted, the pH value is monitored on line in real time through a DCS distributed control system, and the pH value of the reaction environment is controlled to be 8-8.5;
s3, after the total duration reaction time is 180min, the reaction is finished, and the PVP with low residual monomer and low chromaticity is prepared.
Samples were taken and the examined polymeric product PVP had a K value of 31.25, residual order of 7.9ppm and Hazen color of 20.3.
Example 3:
s1, carrying out polymerization under the protection of nitrogen, taking deionized water as a solvent, adding NVP monomer, adding 75 parts of pure water and 45 parts of NVP monomer according to the weight; the pH value is monitored on line in real time by a DCS distributed control system by adopting a pH value interlocking control device, the pH value of the reaction environment is controlled to be 8-8.5, and when the temperature is raised to 50 ℃,35% hydrogen peroxide (35% hydrogen peroxide: NVP monomer=25:1000 by weight) is added;
s2, supplementing hydrogen peroxide (35% hydrogen peroxide: monomer=12:1000 by weight) after the reaction is carried out for 90min, maintaining the reaction temperature at 80-90 ℃, and supplementing hydrogen peroxide (35% hydrogen peroxide: monomer=12:1000 by weight) every 45min, wherein the total supplementing is 3 times; during the period, a pH value interlocking control device is adopted, the pH value is monitored on line in real time through a DCS distributed control system, and the pH value of the reaction environment is controlled to be 8-8.5;
s3, after the total continuous reaction time is 225min, the reaction is finished, and the PVP with low residual monomer and low chromaticity is prepared.
Samples were taken and the examined polymeric product PVP had a K value of=30.28, residual order=5.2 ppm, hazen color=23.4.
Comparative example 1:
referring to the main experimental parameters of example 3, ammonia was periodically detected by PH paper during the reaction, but the PH was not monitored in real time by PH interlock control, and samples were taken after the reaction was completed, and after inspection, the resulting polymerized product PVP had a K value of=30.32, residual order=305 ppm, hazen color=21.1.
Comparative example 2:
aiming at the problem of higher residual monomer in comparative example 1, referring to the main experimental operation of comparative example 1, the number of times of adding hydrogen peroxide is increased from 3 times to 5 times, the total continuous reaction time is prolonged from 225min to 315min, samples are taken after the reaction is finished, and the obtained polymerized product PVP has K value of=30.79, residual monomer of=9.3 ppm and Hazen chroma of=218.5 after inspection.
The experimental results of the above examples 1 to 3 and comparative examples 1 to 2 are summarized in the following table:
| pH range | Temperature range | Total reaction time | K value | Residual sheet | Chromaticity of | |
| Example 1 | 8～8.5 | 50～87.2℃ | 300min | 29.61 | 1.5 | 28.6 |
| Example 2 | 8～8.5 | 50～85.5℃ | 180min | 31.25 | 7.9 | 20.3 |
| Example 3 | 8～8.5 | 50～88.3℃ | 225min | 30.28 | 5.2 | 23.4 |
| Comparative example 1 | 5～9 | 50～87.8℃ | 225min | 30.32 | 305 | 21.1 |
| Comparative example 2 | 5～9 | 50～87.6℃ | 315min | 30.79 | 9.3 | 218.5 |
By comparing the parameters of the embodiment with those of the comparative example, under the condition that the DCS interlocking control device is not adopted to accurately control the pH, both the residual monomer and the chromaticity can not be simultaneously and effectively considered to reach the corresponding indexes. And under the condition of adopting a pH value interlocking control device and accurately controlling the pH value to be between 8 and 8.5, PVP with low residual monomer and low chromaticity can be prepared, and the residual monomer and chromaticity are in accordance with pharmaceutical grade and cosmetic grade indexes.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (6)
1. The preparation method of the PVP with low residual monomer and low chromaticity is characterized in that the method is applied to the preparation of PVP with the K value smaller than 60, and a pH value interlocking control device is adopted, and the pH value of a reaction solution is monitored on line in real time through a DCS distributed control system, so that the pH value of a polymerization environment is ensured to be continuously controlled to be 8-8.5; the method specifically comprises the following steps:
s1, carrying out polymerization reaction at 50-90 ℃ under the protection of nitrogen, taking pure water as a solvent, and adding a certain amount of NVP monomer, hydrogen peroxide and ammonia water;
s2, adding hydrogen peroxide after the reaction is carried out for 60-120 min, and adding hydrogen peroxide every 30-60 min for 2-6 times;
s3, after the total continuous reaction is carried out for 180-300 min, the PVP with low residual monomer and low chromaticity is prepared.
2. The method of claim 1, wherein the reaction temperature is maintained at 80-90 ℃.
3. The method of claim 1, wherein in step S1, pure water is added for the first time with nvp=55 to 135:45, and 35% hydrogen peroxide is added for the first time with NVP monomer=20 to 28:1000.
4. The method of claim 3, wherein the pure water is NVP monomer=68 to 84:45 by weight.
5. The method for preparing low residual monomer low-chromaticity PVP as set forth in claim 1, wherein in step S2, 35% hydrogen peroxide is added to NVP monomer=10-15:1000 by weight each time.
6. The method for preparing low residual monomer low-chromaticity PVP as set forth in claim 1, wherein in step S2, the hydrogen peroxide is added 3-4 times.
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