CN102643377B - Preparation method of homopolymerized N-vinyl butyl lactam iodine with 20% of effective iodine content - Google Patents

Preparation method of homopolymerized N-vinyl butyl lactam iodine with 20% of effective iodine content Download PDF

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CN102643377B
CN102643377B CN201210144313.5A CN201210144313A CN102643377B CN 102643377 B CN102643377 B CN 102643377B CN 201210144313 A CN201210144313 A CN 201210144313A CN 102643377 B CN102643377 B CN 102643377B
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iodine
homopolymerization
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pvp
vinyl butyrate
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CN102643377A (en
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王宇
刘薇
陈占
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Yuang Technology Co.,Ltd.
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SHANGHAI YUKING BIOTECHNOLOGY CO Ltd
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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
    • C08F126/10—N-Vinyl-pyrrolidone
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
    • A61P31/04—Antibacterial agents
    • 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
    • C08F8/00—Chemical modification by after-treatment
    • C08F8/18—Introducing halogen atoms or halogen-containing groups
    • C08F8/20—Halogenation
    • C08F8/22—Halogenation by reaction with free halogens

Abstract

The invention relates to a preparation method of homopolymerized N-vinyl butyl lactam iodine with 20% of effective iodine content, which comprises utilizing N-vinyl butyl lactam homopolymers and iodine with a particle size under 850 mu m as raw materials, wherein the mass ratio of the N-vinyl butyl lactam homopolymers to the iodine with a particle size under 850 mu m is 7:3-5:5; adding 0.01-5.0wt.% of an auxiliary with raw material amount as reference, and reacting with mixing for 5-20 hours at the temperature of 50-100DEG C by means of a sectional preparation method. Preferably, the auxiliary is sodium citrate, sodium chloride or sodium acetate. The preparation method of the homopolymerized N-vinyl butyl lactam iodine with 20% of effective iodine content is ingenious in design and simple in preparation, the effective iodine content of the prepared homopolymerized N-vinyl butyl lactam iodine is 20%, and the prepared homopolymerized N-vinyl butyl lactam iodine has high stability and spectrum bactericidal performance and is suitable for large-scale popularization and application.

Description

The preparation method of the homopolymerization PVP-I of 20% available iodine content
Technical field
The present invention relates to compound preparing technical field, particularly homopolymerization PVP-I preparing technical field, specifically refers to a kind of preparation method of homopolymerization PVP-I of 20% available iodine content.
Background technology
Homopolymerization PVP-I is that yellowish brown is to the amorphous powder of reddish-brown, it is a kind of indefinite form chelated iodine being formed by hydrogen bond and other External Force Actings with the form of complexing by N-vinyl butyrate lactam homopolymer and iodine, a kind of (Cui Yingde of Iodophor, Yi Guobin, Liao Liewen. the synthetic and application [M] of polyvinylpyrrolidone. Science Press, 2001,2:161).It is a kind of outstanding sterilizing agent, and China's nineteen ninety version pharmacopeia starts to record.The sterilizing power that can keep the long period, for the powerful disinfectant of wide spectrum (G & SMED ICAL LTD (US) .Infection fighting composition for topical application[P] .US51377181992:5), virus, bacterium, fungi and mould spores are had to stronger killing action, by Chinese Pharmacopoeia, be approved as the disinfectant that human body can directly be used.N-vinyl butyrate lactam homopolymer is nonionic surface active agent, itself is without anti-microbial effect, but can improve the solubleness of iodine, contribute to improve the wetting and penetrativity of iodine solution to object, the avidity of available iodine cell membrane is strengthened, available iodine can be introduced directly on the cytolemma, tenuigenin of bacterium, kill bacteria immediately in seconds, and then strengthened the sterilizing ability of iodine, PVP-I also has soluble in water simultaneously, to skin, mucous membrane nonirritant, allergy and intoxicating phenomenon, thereby evaluation is very good both at home and abroad.And homopolymerization PVP-I not only can be used as the aqueous solution and use, form that can also solid in some special occasion is employed.Make like this homopolymerization PVP-I be widely used in sterilization, the sterilization of every field, expanded the use range of iodine, at home and abroad in hospital disinfection, be widely used.
The available iodine content of commercially available homopolymerization PVP-I powder available iodine content and pharmacopeia regulation is all at 9%-12% in the market, yet the homopolymerization PVP-I of higher available iodine content is all demonstrating good advantage aspect application aspect or storage, especially aspect the profit of market---the homopolymerization PVP-I thimerosal of the homopolymerization PVP-I that is 10% with available iodine content and 20% homopolymerization PVP-I deallocation same specification processed, available iodine is the cost that 20% homopolymerization PVP-I greatly reduces this thimerosal, also proved its market operability simultaneously.
Therefore, be desirable to provide a kind of preparation method of homopolymerization PVP-I of 20% available iodine content.
Summary of the invention
The object of the invention is to have overcome above-mentioned shortcoming of the prior art, a kind of preparation method of homopolymerization PVP-I of 20% available iodine content is provided, the preparation method of the homopolymerization PVP-I of this 20% available iodine content designs ingenious, preparation is simple, the homopolymerization PVP-I available iodine content of preparing is 20%, also possess higher stability and spectrum bactericidal property simultaneously, be suitable for large-scale promotion application.
To achieve these goals, the preparation method of the homopolymerization PVP-I of 20% available iodine content of the present invention, be characterized in, take N-vinyl butyrate lactam homopolymer and the iodine below 850 μ m particle diameters is raw material, the mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and described 850 μ m particle diameters is 7:3 ~ 5:5, the material quantity of simultaneously take adds the auxiliary agent of 0.01% ~ 5.0% weight percentage as benchmark, and taking sectional type preparation method is stirring reaction 5-20 hour under 50-100 ℃ of condition in temperature.
Described auxiliary agent can be any suitable auxiliary agent, and preferably, described auxiliary agent is Trisodium Citrate, sodium-chlor or sodium-acetate.
The time of the iodine below described N-vinyl butyrate lactam homopolymer, described 850 μ m particle diameters, described auxiliary agent, described temperature, described stirring reaction can be selected from above-mentioned scope, preferably, described N-vinyl butyrate lactam homopolymer is 68g, the iodine of 850 described μ m particle diameters is 32g, the amount of described auxiliary agent is 0.46g, described temperature is 60 ℃, and the time of described stirring reaction is 17 hours.
Described sectional type preparation method refers to first by excessive N-vinyl butyrate lactam homopolymer, a small amount of iodine and auxiliary agent first react for some time, and then supplementary a certain amount of iodine and a small amount of auxiliary agent of adding, homopolymerization N-vinyl butyrate lactam excessive in reactant is continued and Iod R, certainly can also be divided into three sections and even multistage more, more preferably, described sectional type preparation method is first by N-vinyl butyrate lactam homopolymer described in 68g, described in the iodine of 850 μ m particle diameters described in 22g and 0.35g, auxiliary agent was 60 ℃ of stirring reactions 8 hours, add again afterwards auxiliary agent described in the iodine of 850 μ m particle diameters described in 10g and 0.1g to continue stirring reactions 9 hours at 60 ℃.
The time of the iodine below described N-vinyl butyrate lactam homopolymer, described 850 μ m particle diameters, described auxiliary agent, described temperature, described stirring reaction can be selected from above-mentioned scope, preferably, described N-vinyl butyrate lactam homopolymer is 62g, the iodine of 550 described μ m particle diameters is 38g, the amount of described auxiliary agent is 2.6g, described temperature is 75 ℃, and the time of described stirring reaction is 19 hours.
Described sectional type preparation method refers to first by excessive N-vinyl butyrate lactam homopolymer, a small amount of iodine and auxiliary agent first react for some time, and then supplementary a certain amount of iodine and a small amount of auxiliary agent of adding, homopolymerization N-vinyl butyrate lactam excessive in reactant is continued and Iod R, certainly can also be divided into three sections and even multistage more, more preferably, described sectional type preparation method is first by N-vinyl butyrate lactam homopolymer described in 62g, described in the iodine of 550 μ m particle diameters described in 20g and 1.4g, auxiliary agent was 75 ℃ of stirring reactions 11 hours, add again afterwards auxiliary agent described in the iodine of 550 μ m particle diameters described in 18g and 1.2g to continue stirring reactions 8 hours at 75 ℃.
The time of the iodine below described N-vinyl butyrate lactam homopolymer, described 850 μ m particle diameters, described auxiliary agent, described temperature, described stirring reaction can be selected from above-mentioned scope, preferably, described N-vinyl butyrate lactam homopolymer is 70g, the iodine of 750 described μ m particle diameters is 30g, the amount of described auxiliary agent is 0.2g, described temperature is 97 ℃, and the time of described stirring reaction is 19 hours.
Described sectional type preparation method refers to first by excessive N-vinyl butyrate lactam homopolymer, a small amount of iodine and auxiliary agent first react for some time, and then supplementary a certain amount of iodine and a small amount of auxiliary agent of adding, homopolymerization N-vinyl butyrate lactam excessive in reactant is continued and Iod R, certainly can also be divided into three sections and even multistage more, more preferably, described sectional type preparation method is first by N-vinyl butyrate lactam homopolymer described in 70g, described in the iodine of 750 μ m particle diameters described in 30g and 0.15g, auxiliary agent was 97 ℃ of stirring reactions 13 hours, add again afterwards auxiliary agent described in the iodine of 750 μ m particle diameters described in 5g and 0.5g to continue stirring reactions 6 hours at 97 ℃.
Beneficial effect of the present invention is specifically: it is raw material that the preparation method of the homopolymerization PVP-I of 20% available iodine content of the present invention be take N-vinyl butyrate lactam homopolymer and the iodine below 850 μ m particle diameters, the mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and described 850 μ m particle diameters is 7:3 ~ 5:5, the material quantity of simultaneously take adds the auxiliary agent of 0.01% ~ 5.0% weight percentage as benchmark, taking sectional type preparation method is stirring reaction 5-20 hour under 50-100 ℃ of condition in temperature, thereby the homopolymerization PVP-I available iodine content obtaining is more than 20%, design ingenious, preparation is simple, also possess higher stability and spectrum bactericidal property simultaneously, be suitable for large-scale promotion application.
Accompanying drawing explanation
Fig. 1 is the influence curve figure of temperature of reaction to available iodine content.
Fig. 2 is that auxiliary agent adds the influence curve figure to the reaction times.
Fig. 3 is the influence curve figure to available iodine content that adds of auxiliary agent.
Fig. 4 is the influence curve figure of the particle diameter of iodine to available iodine content.
Embodiment
In order more clearly to understand technology contents of the present invention, especially exemplified by following examples, describe in detail.
1.1 experimental raw
Table 1 main raw material
Figure BDA00001622529900031
Figure BDA00001622529900041
1.2 experimental instrument and equipment
250ml there-necked flask, HH-WO thermostatical oil bath, S312 electric mixer, FA2004 analytical balance, Erlenmeyer flask, 10mLl transfer pipet, base buret.
The mensuration of 1.3 available iodine contents
The available iodine concentration of sample can with reference to Chinese Pharmacopoeia (Chinese Pharmacopoeia. two [S] .2005:823) method measures concentration.This experiment adopts American Pharmacopeia to survey its available iodine content: take the about 1g of sample, the accurately weighed beaker that is placed in, adding appropriate stirring of water all proceeds in 100mL volumetric flask it after dissolving, by transfer pipet precision, measure 2 parts of sample solution 20mL to iodine flask, with Sulfothiorine titrand (0.1mol/L) titration, the nearly appropriate amount of starch indicator that drips when faint yellow continues to drop to blue disappearance with Sulfothiorine, records the volume of Sulfothiorine used the available iodine content of calculation sample.
In sample, available iodine content w represents with massfraction (%):
w = ( V 1 - V 2 ) × 12.69 ÷ 1000 m × 100
In formula:
V 1---sample consumes the volume of sodium thiosulfate standard solution, and unit is milliliter (mL);
V 2---the volume of the sodium thiosulfate standard solution that blank test consumes, unit is milliliter (mL);
M---the quality of institute's sample thief, unit is gram (g).
2 results and discussion
The 2.1 always impacts on available iodine by iodine amount
The maximum available iodine content of homopolymerization PVP-I is subject to the restriction of solubleness, in order always to reduce, by iodine amount, reduces product cost, need to find out the rational proportion of homopolymerization N-vinyl butyrate lactam and iodine.
Table 2: the always impact on available iodine by iodine amount
Figure BDA00001622529900043
Figure BDA00001622529900051
From table 2 data, in homopolymerization PVP-I available iodine content within the specific limits with increasing with the increase of iodine amount, reach certain content after numerical value tend towards stability.Reason may be homopolymerization N-vinyl butyrate lactam molecular chain end group quantity limitation the amount of its institute's chelated iodine.Available iodine content be in 20% homopolymerization PVP-I raw material always by iodine amount 30% ~ 50% for best.
The impact of 2.2 temperature on available iodine content
Both can there is complexing in N-vinyl butyrate lactam homopolymer and iodine, but the available iodine content of required asynchronism(-nization) under differing temps, the finished product also different at normal temperatures, and general temperature of reaction is controlled at 45-100 ℃.At homopolymerization N-vinyl butyrate lactam massfraction, be 70%, the massfraction of iodine is 30%, and identical auxiliary agent reacts 6 hours, and the impact of research temperature on product available iodine content, is shown in Fig. 1.
From Fig. 1, data can be found out, 70 ℃ of optimum tempss for preparation homopolymerization PVP-I; Meanwhile, under the same conditions, the available iodine content of PVP-I is along with the rising of temperature first raises and reduces afterwards.This is mainly because the rising of temperature is conducive to improve the activated molecule number of reactant, thereby accelerates intermolecular collision frequency, and reactant is fully reacted; But excess Temperature reaction rate accelerates, in this reaction process, available iodine content climax time of occurrence is significantly shifted to an earlier date, and along with the prolongation in reaction times, the complex bonds between homopolymerization N-vinyl butyrate lactam and iodine ruptures gradually, available iodine content declines rapidly.
2.3 add the impact of auxiliary agent on available iodine content
Get the massfraction 70% of homopolymerization N-vinyl butyrate lactam, under 30%, 70 ℃ of condition of massfraction of iodine, react, by adding the auxiliary agents such as Trisodium Citrate to investigate the impact on reaction times (Fig. 2) and available iodine content (Fig. 3) that adds of auxiliary agent:
As can be seen from Figures 2 and 3, the auxiliary agents such as Trisodium Citrate add Reaction time shorten greatly, also can effectively improve maximum available iodine content in reaction simultaneously, its optimal addn is raw material 1.0%.The auxiliary agents such as Trisodium Citrate add the grinding aid effect of playing, has promoted contacting between iodine and homopolymerization N-vinyl butyrate lactam to make internal friction aggravation, thereby caused reaction rate accelerates, complex reaction abundant, and then the reaction times reduces, available iodine content raises.
The impact of the processing of 2.4 raw materials on available iodine content
The massfraction of getting N-vinyl butyrate lactam is 70%, and the massfraction of iodine is to react 12 hours under 30%, 70 ℃ of condition, and the impact of the iodine of research different-grain diameter on product available iodine content, is shown in Fig. 4.
The reaction essence of homopolymerization N-vinyl butyrate lactam and iodine is solid-solid reaction and the gas-solid reaction of iodine and homopolymerization N-vinyl butyrate lactam.Raw material iodine is carried out after particle diameter processing, can greatly improve the contact surface of iodine and homopolymerization N-vinyl butyrate lactam, thereby improve the influencing factors of quality in speed of reaction and available iodine content reduction reaction times and reaction process.This is mainly because the strong oxidizing property of iodine, if long iodine of reaction times can cause certain oxidation to make its molecular rupture to N-vinyl butyrate lactam, affects the carrying out of complex reaction; As can be seen here the processing of raw material iodine particle diameter is absolutely necessary, from Fig. 4, can be confirmed.
2.5 impacts of sectional type preparation technology on available iodine content
Sectional type preparation: first use excessive ceridust base butyrolactam and a small amount of iodine, under the promoter effects such as sodium-chlor, complexing generates the homopolymerization PVP-I of lower available iodine content (12%-18%), and then the supplementary auxiliary agents such as a certain amount of iodine and a small amount of sodium-chlor that add, homopolymerization N-vinyl butyrate lactam excessive in reactant is continued and Iod R, thereby prepare the homopolymerization PVP-I of high available iodine content (more than 20%).
This method and the tradition preparation technology that once feeds intake compares, and the available iodine content of the homopolymerization PVP-I that it is prepared is higher, generally more than 20%.Reason may be: on the one hand, the complex performance of iodine is fine, is easy to prepare the homopolymerization PVP-I of 8%-12% available iodine content under general condition; But, because homopolymerization N-vinyl butyrate lactam self end group limited amount adds on molecular chain that between each group, steric hindrance is larger, make it be difficult to reach theoretic abundant complexing with iodine.Traditional technology that Here it is cannot be made the reason of high-content homopolymerization PVP-I.On the other hand, this sectional type preparation technology has overcome homopolymerization N-vinyl butyrate lactam and for a long time in reaction process, is being subject to temperature and iodine strong oxidizing property deactivation.The complexation process of homopolymerization N-vinyl butyrate lactam and iodine belongs to typical thermopositive reaction, in reaction process, can emit more heat transfer, can temperature of reaction system be raise in the short period, thereby cause homopolymerization N-vinyl butyrate lactam partially denaturing inactivation; And prepare because " reflecting point " in whole process is less by sectional type, relatively less can also comparatively fast the shedding of heat producing, simultaneously, owing to effectively having reduced the steric hindrance of each group of homopolymerization N-vinyl butyrate lactam molecular chain adding of the auxiliary agents such as sodium-chlor, thereby greatly improve complexing degree, prepare the homopolymerization PVP-I of higher available iodine content.
3 conclusions
The ingredient proportion of homopolymerization N-vinyl butyrate lactam and iodine of take is 7:3 ~ 5:5, by to temperature of reaction, the particle diameter of auxiliary agent and iodine regulates control, develop a set of actual production high, operational condition is gentle, cost is low, the solid phase heating means of take are prepared the production technique of 20% available iodine content homopolymerization PVP-I: the massfraction of homopolymerization N-vinyl butyrate lactam is 50% ~ 70%, iodine quality mark below 850 μ m particle diameters is 50% ~ 30%, promoter addition is 0.01% ~ 5.0% of material quantity, the available iodine content of the homopolymerization PVP-I of preparing by stepwise process stirring reaction under 50 ℃ ~ 100 ℃ conditions is more than 20%.
Enumerate several embodiment below and be described more specifically the present invention, but the present invention is not subject to the restriction of these embodiment.In content below, unless specified otherwise is only expressed as " % " by " % by weight ".
Embodiment 1
Take the homopolymerization N-vinyl butyrate lactam K30 that 60g Shanghai Yu'ang Chemical Technology Development Co., Ltd. produces, particle diameter is the iodine 22g of 850 μ m, 0.35g Trisodium Citrate joins in 500ml there-necked flask, inserting stirring rake stirring at low speed mixes raw material, then put into 50 ℃ of oil bath stirring heating reactions 8 hours, adding afterwards particle diameter is iodine 18g and the 0.1g Trisodium Citrate of 850 μ m again, and continuing heated and stirred reaction, cooling after 9 hours to sieve and obtain available iodine content be 21.11% homopolymerization PVP-I.
Comparative example 1:
Except adding citric acid sodium not, carry out the operation same with embodiment 1, it is 15.72% that result detects available iodine content.
Embodiment 2:
Take the homopolymerization N-vinyl butyrate lactam K30 that 50g Shanghai Yu'ang Chemical Technology Development Co., Ltd. produces, particle diameter is the iodine 25g of 550 μ m, 2.6g sodium-acetate joins in 500ml there-necked flask, inserting stirring rake stirring at low speed mixes raw material, then put into 75 ℃ of oil bath stirring heating reactions 11 hours, adding afterwards particle diameter is iodine 25g and the 2.4g sodium-acetate of 550 μ m again, and continuing heated and stirred reaction, cooling after 9 hours to sieve and obtain available iodine content be 21.63% homopolymerization PVP-I.
Comparative example 2:
Except using, without the iodine (particle diameter is greater than 1500 μ m) of pulverizing, to replace particle diameter be the iodine of 550 μ m, carries out the operation same with embodiment 2, and result detects available iodine content 16.22%.
Embodiment 3
Take the homopolymerization N-vinyl butyrate lactam K30 that 70g Shanghai Yu'ang Chemical Technology Development Co., Ltd. produces, particle diameter is the iodine 25g of 750 μ m, 0.005g sodium-chlor joins in 500ml there-necked flask, inserting stirring rake stirring at low speed mixes raw material, then put into 100 ℃ of oil bath stirring heating reactions 3 hours, adding afterwards particle diameter is iodine 5g and the 0.005g sodium-chlor of 750 μ m again, and continuing heated and stirred reaction, cooling after 2 hours to sieve and obtain available iodine content be 20.05% homopolymerization PVP-I.
Comparative example 3:
Take the homopolymerization N-vinyl butyrate lactam K30 that 70g Shanghai Yu'ang Chemical Technology Development Co., Ltd. produces, particle diameter is the iodine 30g of 750 μ m, 0.1g sodium-acetate joins in 500ml there-necked flask, inserting stirring rake stirring at low speed mixes raw material, then put into 100 ℃ of oil bath stirring heating reaction 5 hours, coolingly sieve to such an extent that available iodine content is 17.83% homopolymerization PVP-I.
It is 7:3 ~ 5:5 that raw material N-vinyl butyrate lactam homopolymer and the iodine quality ratio after particle diameter select to be processed are take in the present invention, the material quantity of simultaneously take adds the auxiliary agent (Trisodium Citrate, sodium-chlor, sodium-acetate) of 0.01% ~ 5.0% weight as benchmark, take sectional type preparation method about stirring reaction 5-20 hour, to obtain the homopolymerization PVP-I powder of high available iodine content under 50-100 ℃ of condition.
To sum up, the preparation method of the homopolymerization PVP-I of 20% available iodine content of the present invention designs ingenious, preparation is simple, the homopolymerization PVP-I available iodine content of preparing is 20%, also possess higher stability and spectrum bactericidal property simultaneously, be suitable for large-scale promotion application.
In this specification sheets, the present invention is described with reference to its specific embodiment.But, still can make various modifications and conversion obviously and not deviate from the spirit and scope of the present invention.Therefore, specification sheets and accompanying drawing are regarded in an illustrative, rather than a restrictive.

Claims (6)

1. the preparation method of the homopolymerization PVP-I of an available iodine content, it is characterized in that, take N-vinyl butyrate lactam homopolymer and the iodine below 850 μ m particle diameters is raw material, the mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and described 850 μ m particle diameters is 7:3～5:5, the material quantity of simultaneously take adds the auxiliary agent of 0.01%～5.0% weight percentage as benchmark, and taking sectional type preparation method is stirring reaction 5-20 hour under 50-100 ℃ of condition in temperature.
2. the preparation method of the homopolymerization PVP-I of 20% available iodine content according to claim 1, is characterized in that, described auxiliary agent is Trisodium Citrate, sodium-chlor or sodium-acetate.
3. the preparation method of the homopolymerization PVP-I of 20% available iodine content according to claim 1, it is characterized in that, described N-vinyl butyrate lactam homopolymer is 68g, the iodine of 850 described μ m particle diameters is 32g, the amount of described auxiliary agent is 0.46g, described temperature is 60 ℃, and the time of described stirring reaction is 17 hours.
4. the preparation method of the homopolymerization PVP-I of 20% available iodine content according to claim 1, it is characterized in that, described N-vinyl butyrate lactam homopolymer is 62g, the iodine of 550 described μ m particle diameters is 38g, the amount of described auxiliary agent is 2.6g, described temperature is 75 ℃, and the time of described stirring reaction is 19 hours.
5. the preparation method of the homopolymerization PVP-I of 20% available iodine content according to claim 4, it is characterized in that, described sectional type preparation method be first by auxiliary agent described in the iodine of 550 μ m particle diameters described in N-vinyl butyrate lactam homopolymer, 20g described in 62g and 1.4g 75 ℃ of stirring reactions 11 hours, add again afterwards auxiliary agent described in the iodine of 550 μ m particle diameters described in 18g and 1.2g to continue stirring reactions 8 hours at 75 ℃.
6. the preparation method of the homopolymerization PVP-I of 20% available iodine content according to claim 1, it is characterized in that, described N-vinyl butyrate lactam homopolymer is 70g, the iodine of 750 described μ m particle diameters is 30g, the amount of described auxiliary agent is 0.2g, described temperature is 97 ℃, and the time of described stirring reaction is 19 hours.
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