CN102643377A - 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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CN102643377A
CN102643377A CN2012101443135A CN201210144313A CN102643377A CN 102643377 A CN102643377 A CN 102643377A CN 2012101443135 A CN2012101443135 A CN 2012101443135A CN 201210144313 A CN201210144313 A CN 201210144313A CN 102643377 A CN102643377 A CN 102643377A
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iodine
vinyl butyrate
butyrate lactam
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homopolymerization
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CN102643377B (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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    • 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
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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 N-vinyl butyrate lactam iodine of 20% available iodine content
Technical field
The present invention relates to the compound technical field, particularly homopolymerization N-vinyl butyrate lactam iodine preparing technical field specifically is meant a kind of preparation method of homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content.
Background technology
Homopolymerization N-vinyl butyrate lactam iodine is the amorphous powder of yellowish brown to reddish-brown; It is a kind of indefinite form chelated iodine that forms by hydrogen bond and other external force effects with the form of complexing by N-vinyl butyrate lactam homopolymer and iodine; Be Iodophor a kind of (Cui Yingde, Yi Guobin, Liao Liewen. Vinylpyrrolidone polymer synthetic with use [M]. Science Press; 2001,2:161).It is a kind of outstanding sterilizing agent, and China's nineteen ninety version pharmacopeia begins to record.The sterilizing power that can keep the long period; Powerful disinfectant (G&SMED ICAL LTD (US) .Infection fighting composition for topical application [P] .US51377181992:5) for wide spectrum; Virus, bacterium, fungi and mould spores all there are stronger killing action, are ratified the disinfectant that can directly use by Chinese Pharmacopoeia for human body.N-vinyl butyrate lactam homopolymer is a non-ionics, no antibiotic effect own, but can put forward periodic solubleness; Help to improve the wetting and penetrativity of iodine solution to object; Make the avidity of available iodine cell membrane strengthen, can available iodine be introduced directly on the cytolemma, tenuigenin of bacterium, in seconds kill bacteria immediately; And then strengthened the sterilizing ability of iodine; While N-vinyl butyrate lactam iodine also has soluble in water, and to skin, mucous membrane nonirritant, allergy and intoxicating phenomenon, thereby evaluation is very good both at home and abroad.And homopolymerization N-vinyl butyrate lactam iodine not only can be used as the aqueous solution and uses, and can also the solid form be employed in some special occasion.Make homopolymerization N-vinyl butyrate lactam iodine be widely used in sterilization, the sterilization of every field like this, expanded the use range of iodine, at home and abroad be widely used in the hospital disinfection.
The available iodine content of commercially available in the market homopolymerization N-vinyl butyrate lactam iodine powder available iodine content and pharmacopeia regulation is all at 9%-12%; Yet the homopolymerization N-vinyl butyrate lactam iodine of higher available iodine content still is all to demonstrate good advantage aspect the storage in application facet; Especially aspect the profit of market---using available iodine content is the homopolymerization N-vinyl butyrate lactam iodine thimerosal of the homopolymerization N-vinyl butyrate lactam iodine deallocation system of 10% homopolymerization N-vinyl butyrate lactam iodine and 20% with a kind of specification; Available iodine is the cost that 20% homopolymerization N-vinyl butyrate lactam iodine greatly reduces this thimerosal, has also proved its market operability simultaneously.
Therefore, be desirable to provide a kind of preparation method of homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content.
Summary of the invention
The objective of the invention is to have overcome above-mentioned shortcoming of the prior art; A kind of preparation method of homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content is provided; The preparation method of the homopolymerization N-vinyl butyrate lactam iodine of this 20% available iodine content designs ingenious, and preparation is simple, and the homopolymerization N-vinyl butyrate lactam iodine available iodine content of preparing is 20%; Also possess advantages of higher stability and spectrum bactericidal property simultaneously, be suitable for large-scale promotion application.
To achieve these goals; The preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content of the present invention; Be characterized in; With N-vinyl butyrate lactam homopolymer and the iodine below the 850 μ m particle diameters is raw material; The mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and the described 850 μ m particle diameters is 7:3 ~ 5:5, is the auxiliary agent that benchmark adds 0.01% ~ 5.0% weight percentage with the material quantity simultaneously, and taking the sectional preparation method is under the 50-100 ℃ of condition stirring reaction 5-20 hour in temperature.
Said auxiliary agent can be any proper auxiliary agent, and preferably, said auxiliary agent is Trisodium Citrate, sodium-chlor or sodium-acetate.
The time of the iodine below said N-vinyl butyrate lactam homopolymer, the described 850 μ m particle diameters, said auxiliary agent, said temperature, said stirring reaction can be selected from above-mentioned scope; Preferably; Said N-vinyl butyrate lactam homopolymer is 68g, and the iodine of described 850 μ m particle diameters is 32g, and the amount of said auxiliary agent is 0.46g; Said temperature is 60 ℃, and the time of said stirring reaction is 17 hours.
Said sectional preparation method refers to earlier excessive N-vinyl butyrate lactam homopolymer, a spot of iodine and auxiliary agent is reacted for some time earlier; And then additional a certain amount of iodine and the little auxiliary of adding; Homopolymerization N-vinyl butyrate lactam excessive in the reactant is continued and Iod R; Certainly can also be divided into three sections and even multistage more; More preferably, said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 68g homopolymer, the described 850 μ m particle diameters of 22g and the said auxiliary agent of 0.35g 60 ℃ of stirring reactions 8 hours, the iodine and the said auxiliary agent of 0.1g that add the described 850 μ m particle diameters of 10g afterwards again continued stirring reactions 9 hours at 60 ℃.
The time of the iodine below said N-vinyl butyrate lactam homopolymer, the described 850 μ m particle diameters, said auxiliary agent, said temperature, said stirring reaction can be selected from above-mentioned scope; Preferably; Said N-vinyl butyrate lactam homopolymer is 62g, and the iodine of described 550 μ m particle diameters is 38g, and the amount of said auxiliary agent is 2.6g; Said temperature is 75 ℃, and the time of said stirring reaction is 19 hours.
Said sectional preparation method refers to earlier excessive N-vinyl butyrate lactam homopolymer, a spot of iodine and auxiliary agent is reacted for some time earlier; And then additional a certain amount of iodine and the little auxiliary of adding; Homopolymerization N-vinyl butyrate lactam excessive in the reactant is continued and Iod R; Certainly can also be divided into three sections and even multistage more; More preferably, said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 62g homopolymer, the described 550 μ m particle diameters of 20g and the said auxiliary agent of 1.4g 75 ℃ of stirring reactions 11 hours, the iodine and the said auxiliary agent of 1.2g that add the described 550 μ m particle diameters of 18g afterwards again continued stirring reactions 8 hours at 75 ℃.
The time of the iodine below said N-vinyl butyrate lactam homopolymer, the described 850 μ m particle diameters, said auxiliary agent, said temperature, said stirring reaction can be selected from above-mentioned scope; Preferably; Said N-vinyl butyrate lactam homopolymer is 70g, and the iodine of described 750 μ m particle diameters is 30g, and the amount of said auxiliary agent is 0.2g; Said temperature is 97 ℃, and the time of said stirring reaction is 19 hours.
Said sectional preparation method refers to earlier excessive N-vinyl butyrate lactam homopolymer, a spot of iodine and auxiliary agent is reacted for some time earlier; And then additional a certain amount of iodine and the little auxiliary of adding; Homopolymerization N-vinyl butyrate lactam excessive in the reactant is continued and Iod R; Certainly can also be divided into three sections and even multistage more; More preferably, said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 70g homopolymer, the described 750 μ m particle diameters of 30g and the said auxiliary agent of 0.15g 97 ℃ of stirring reactions 13 hours, the iodine and the said auxiliary agent of 0.5g that add the described 750 μ m particle diameters of 5g afterwards again continued stirring reactions 6 hours at 97 ℃.
Beneficial effect of the present invention specifically is: the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content of the present invention is a raw material with N-vinyl butyrate lactam homopolymer and the iodine below the 850 μ m particle diameters; The mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and the described 850 μ m particle diameters is 7:3 ~ 5:5; Be the auxiliary agent that benchmark adds 0.01% ~ 5.0% weight percentage simultaneously with the material quantity; Taking the sectional preparation method is under the 50-100 ℃ of condition stirring reaction 5-20 hour in temperature; Thereby the homopolymerization N-vinyl butyrate lactam iodine available iodine content that obtains is more than 20%, designs ingeniously, and preparation is simple; Also possess advantages of higher stability and spectrum bactericidal property simultaneously, be suitable for large-scale promotion application.
Description of drawings
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 of the adding of auxiliary agent to available iodine content.
Fig. 4 is the influence curve figure of the particle diameter of iodine to available iodine content.
Embodiment
In order more to be expressly understood technology contents of the present invention, the special following examples of lifting specify.
1.1 experimental raw
Table 1 main raw material
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.
1.3 the mensuration of available iodine content
The available iodine concentration of sample can with reference to Chinese Pharmacopoeia (Chinese Pharmacopoeia. two [S] .2005:823) method measures concentration.This experiment adopts USP to survey its available iodine content: take by weighing the about 1g of sample; The accurate fixation of claiming is in beaker; Add an amount of stirring of water it is all changed in the 100mL volumetric flask after the dissolving, measure 2 parts of sample solution 20mL to iodine flask, with Sulfothiorine titrand (0.1mol/L) titration with the transfer pipet precision; The nearly appropriate amount of starch indicator that drips when faint yellow continues to drip to blueness with Sulfothiorine and disappears, and writes down the volume of used Sulfothiorine and the available iodine content of calculation sample.
Available iodine content w representes with massfraction (%) in the sample:
w = ( V 1 - V 2 ) × 12.69 ÷ 1000 m × 100
In the formula:
V 1---sample consumes the volume of sodium thiosulfate standard solution, and unit is a milliliter (mL);
V 2---the volume of the sodium thiosulfate standard solution that blank test consumes, unit are milliliter (mL);
M---the quality of institute's sample thief, unit is gram (g).
2 results and discussion
2.1 always with of the influence of iodine amount to available iodine
The maximum available iodine content of homopolymerization N-vinyl butyrate lactam iodine receives the restriction of solubleness, reduces product cost in order always to reduce with the iodine amount, need find out the rational proportion of homopolymerization N-vinyl butyrate lactam and iodine.
Table 2: always with of the influence of iodine amount to available iodine
Figure BDA00001622529900043
Figure BDA00001622529900051
Can know from table 2 data, in the homopolymerization N-vinyl butyrate lactam iodine available iodine content within the specific limits with increasing with iodometric increase, reach certain content after numerical value tend towards stability.Reason possibly be homopolymerization N-vinyl butyrate lactam molecular chain the end group quantity limitation amount of its institute's chelated iodine.Available iodine content be in 20% the homopolymerization N-vinyl butyrate lactam iodine raw material always with iodine amount 30% ~ 50% for best.
2.2 temperature is to the influence of available iodine content
Complexing both can take place in N-vinyl butyrate lactam homopolymer and iodine at normal temperatures, but the available iodine content of required asynchronism(-nization) under the differing temps, the finished product is also different, and general temperature of reaction is controlled at 45-100 ℃.At homopolymerization N-vinyl butyrate lactam massfraction is 70%, and the massfraction of iodine is 30%, and identical auxiliary agent reacted 6 hours, and the research temperature is seen Fig. 1 to the influence of product available iodine content.
Data can be found out from Fig. 1,70 ℃ of optimum tempss for preparation homopolymerization N-vinyl butyrate lactam iodine; Simultaneously, under the same conditions, the available iodine content of N-vinyl butyrate lactam iodine is along with first rising of the rising of temperature afterwards reduced.This mainly is because the rising of temperature helps improving the activated molecule number of reactant, thereby accelerates intermolecular collision frequency, and reactant is fully reacted; But the too high reaction rate accelerates of temperature, available iodine content climax time of occurrence is significantly shifted to an earlier date in this reaction process, and along with the prolongation in reaction times, the complex bonds between homopolymerization N-vinyl butyrate lactam and the iodine ruptures gradually, available iodine content descends rapidly.
2.3 add the influence of auxiliary agent to available iodine content
Get the massfraction 70% of homopolymerization N-vinyl butyrate lactam, react under 30%, 70 ℃ of condition of the massfraction of iodine, investigate the influence of the adding of auxiliary agent reaction times (Fig. 2) and available iodine content (Fig. 3) through adding auxiliary agents such as Trisodium Citrate:
Can find out that from Fig. 2 and Fig. 3 the adding of auxiliary agents such as Trisodium Citrate can be shortened the reaction times greatly, also can effectively improve maximum available iodine content in the reaction simultaneously, its optimal addn is 1.0% of a raw material.The grinding aid effect is played in the adding of auxiliary agents such as Trisodium Citrate, has promoted contacting between iodine and the homopolymerization N-vinyl butyrate lactam to make the internal friction aggravation, thereby causes reaction rate accelerates, complex reaction abundant, and then the reaction times reduces, available iodine content raises.
2.4 the processing of raw material is to the influence of available iodine content
The massfraction of getting the N-vinyl butyrate lactam is 70%, and the massfraction of iodine is to react 12 hours under 30%, 70 ℃ of condition, and the iodine of research different-grain diameter is seen Fig. 4 to the influence of product available iodine content.
The reaction essence of homopolymerization N-vinyl butyrate lactam and iodine is the solid-solid reaction and the gas-solid reaction of iodine and homopolymerization N-vinyl butyrate lactam.Raw material iodine is carried out can improving the contact surface of iodine and homopolymerization N-vinyl butyrate lactam greatly, thereby improving the influencing factors of quality in speed of reaction and available iodine content reduction reaction times and the reaction process after particle diameter handles.This mainly is because the strong oxidizing property of iodine if long iodine of reaction times can cause certain oxidation to make its molecular rupture to the N-vinyl butyrate lactam, influences the carrying out of complex reaction; This shows that the processing to raw material iodine particle diameter is absolutely necessary, and can be confirmed from Fig. 4.
2.5 sectional preparation technology is to the influence of available iodine content
Sectional preparation: earlier with excessive ceridust base butyrolactam and a spot of iodine; Complexing generates the homopolymerization N-vinyl butyrate lactam iodine of low available iodine content (12%-18%) under promoter effects such as sodium-chlor; And then the additional auxiliary agents such as a certain amount of iodine and little sodium chloride that add; Homopolymerization N-vinyl butyrate lactam excessive in the reactant is continued and Iod R, thereby prepare the homopolymerization N-vinyl butyrate lactam iodine of high available iodine content (more than 20%).
This method is compared with traditional one feeding preparation technology, and the available iodine content of the homopolymerization N-vinyl butyrate lactam iodine that it is prepared is higher, generally more than 20%.Reason maybe for: on the one hand, the complex performance of iodine is fine, is easy to prepare the homopolymerization N-vinyl butyrate lactam iodine of 8%-12% available iodine content under the general condition; But,, make it be difficult to reach theoretic abundant complexing with iodine because homopolymerization N-vinyl butyrate lactam self end group limited amount adds on the molecular chain that steric hindrance is bigger between each group.Traditional technology that Here it is can't be made the reason of high-content homopolymerization N-vinyl butyrate lactam iodine.On the other hand, this sectional preparation technology has overcome homopolymerization N-vinyl butyrate lactam and is for a long time receiving temperature and iodine strong oxidizing property sex change inactivation in the reaction process.The complexing process of homopolymerization N-vinyl butyrate lactam and iodine belongs to typical thermopositive reaction, can emit more heat transfer in the reaction process, can temperature of reaction system raise in the short period, thereby cause homopolymerization N-vinyl butyrate lactam partially denaturing inactivation; And it is less through the sectional preparation owing to " reflecting point " in the whole process; Less relatively can also comparatively fast the shedding of heat that produces; Simultaneously; Because the adding of auxiliary agents such as sodium-chlor has reduced the steric hindrance of each group of homopolymerization N-vinyl butyrate lactam molecular chain effectively, thereby improves the complexing degree greatly, prepares the homopolymerization N-vinyl butyrate lactam iodine of higher available iodine content.
3 conclusions
Ingredient proportion with homopolymerization N-vinyl butyrate lactam and iodine is 7:3 ~ 5:5; Through the particle diameter of temperature of reaction, auxiliary agent and iodine is regulated control; Develop that a cover actual production property is high, operational condition is gentle, cost is low; The production technique for preparing 20% available iodine content homopolymerization N-vinyl butyrate lactam iodine with the solid phase heating means: the massfraction of homopolymerization N-vinyl butyrate lactam is 50% ~ 70%; Iodine quality mark below the 850 μ m particle diameters is 50% ~ 30%, and promoter addition is 0.01% ~ 5.0% of a material quantity, and the available iodine content of the homopolymerization N-vinyl butyrate lactam iodine of under 50 ℃ ~ 100 ℃ conditions, preparing through the stepwise process stirring reaction is more than 20%.
Enumerate several embodiment below the present invention more specifically is described, but the present invention does not receive the restriction of these embodiment.In the content below, only if specified otherwise only is expressed as " % " with " weight % ".
Embodiment 1
Take by weighing 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 the 500ml there-necked flask; Inserting the stirring rake stirring at low speed makes raw materials mix even; Put into 50 ℃ of oil bath stirring heating reaction 8 hours then, adding particle diameter afterwards again is iodine 18g and the 0.1g Trisodium Citrate of 850 μ m, continues heated and stirred and reacts 9 hours postcooling and sieve that promptly to get available iodine content be 21.11% homopolymerization N-vinyl butyrate lactam iodine.
Comparative Examples 1:
Except not the adding citric acid sodium, carry out the operation same with embodiment 1, it is 15.72% that the result detects available iodine content.
Embodiment 2:
Take by weighing 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 the 500ml there-necked flask; Inserting the stirring rake stirring at low speed makes raw materials mix even; Put into 75 ℃ of oil bath stirring heating reaction 11 hours then, adding particle diameter afterwards again is iodine 25g and the 2.4g sodium-acetate of 550 μ m, continues heated and stirred and reacts 9 hours postcooling and sieve that promptly to get available iodine content be 21.63% homopolymerization N-vinyl butyrate lactam iodine.
Comparative Examples 2:
To replace particle diameter without the iodine of pulverizing (particle diameter is greater than 1500 μ m) is the iodine of 550 μ m except using, and carries out the operation same with embodiment 2, and the result detects available iodine content 16.22%.
Embodiment 3
Take by weighing 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 the 500ml there-necked flask; Inserting the stirring rake stirring at low speed makes raw materials mix even; Put into 100 ℃ of oil bath stirring heating reaction 3 hours then, adding particle diameter afterwards again is iodine 5g and the 0.005g sodium-chlor of 750 μ m, continues heated and stirred and reacts 2 hours postcooling and sieve that promptly to get available iodine content be 20.05% homopolymerization N-vinyl butyrate lactam iodine.
Comparative Examples 3:
Take by weighing 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 the 500ml there-necked flask; Insert the stirring rake stirring at low speed and make raw materials mix even, put into 100 ℃ of oil bath stirring heating reactions 5 hours then, cooling is sieved to such an extent that available iodine content is 17.83% homopolymerization N-vinyl butyrate lactam iodine.
Iodine quality ratio after the present invention selects to handle with raw material N-vinyl butyrate lactam homopolymer with through particle diameter is 7:3 ~ 5:5; Be the auxiliary agent (Trisodium Citrate, sodium-chlor, sodium-acetate) that benchmark adds 0.01% ~ 5.0% weight simultaneously with the material quantity; Take the sectional preparation method under the 50-100 ℃ of condition about stirring reaction 5-20 hour, promptly obtain the homopolymerization N-vinyl butyrate lactam iodine powder of high available iodine content.
To sum up; The preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content of the present invention designs ingenious; Preparation is simple; The homopolymerization N-vinyl butyrate lactam iodine available iodine content of preparing is 20%, also possesses advantages of higher stability and spectrum bactericidal property simultaneously, is suitable for large-scale promotion application.
In this specification sheets, the present invention is described with reference to its certain embodiments.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 (8)

1. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of an available iodine content; It is characterized in that; With N-vinyl butyrate lactam homopolymer and the iodine below the 850 μ m particle diameters is raw material; The mass ratio of the iodine below wherein said N-vinyl butyrate lactam homopolymer and the described 850 μ m particle diameters is 7:3 ~ 5:5, is the auxiliary agent that benchmark adds 0.01% ~ 5.0% weight percentage with the material quantity simultaneously, and taking the sectional preparation method is under the 50-100 ℃ of condition stirring reaction 5-20 hour in temperature.
2. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 1 is characterized in that said auxiliary agent is Trisodium Citrate, sodium-chlor or sodium-acetate.
3. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 1; It is characterized in that; Said N-vinyl butyrate lactam homopolymer is 68g, and the iodine of described 850 μ m particle diameters is 32g, and the amount of said auxiliary agent is 0.46g; Said temperature is 60 ℃, and the time of said stirring reaction is 17 hours.
4. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 3; It is characterized in that; Said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 68g homopolymer, the described 850 μ m particle diameters of 22g and the said auxiliary agent of 0.35g 60 ℃ of stirring reactions 8 hours, the iodine and the said auxiliary agent of 0.1g that add the described 850 μ m particle diameters of 10g afterwards again continued stirring reactions 9 hours at 60 ℃.
5. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 1; It is characterized in that; Said N-vinyl butyrate lactam homopolymer is 62g, and the iodine of described 550 μ m particle diameters is 38g, and the amount of said auxiliary agent is 2.6g; Said temperature is 75 ℃, and the time of said stirring reaction is 19 hours.
6. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 5; It is characterized in that; Said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 62g homopolymer, the described 550 μ m particle diameters of 20g and the said auxiliary agent of 1.4g 75 ℃ of stirring reactions 11 hours, the iodine and the said auxiliary agent of 1.2g that add the described 550 μ m particle diameters of 18g afterwards again continued stirring reactions 8 hours at 75 ℃.
7. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 1; It is characterized in that; Said N-vinyl butyrate lactam homopolymer is 70g, and the iodine of described 750 μ m particle diameters is 30g, and the amount of said auxiliary agent is 0.2g; Said temperature is 97 ℃, and the time of said stirring reaction is 19 hours.
8. the preparation method of the homopolymerization N-vinyl butyrate lactam iodine of 20% available iodine content according to claim 7; It is characterized in that; Said sectional preparation method be at first with the iodine of the said N-vinyl butyrate lactam of 70g homopolymer, the described 750 μ m particle diameters of 30g and the said auxiliary agent of 0.15g 97 ℃ of stirring reactions 13 hours, the iodine and the said auxiliary agent of 0.5g that add the described 750 μ m particle diameters of 5g afterwards again continued stirring reactions 6 hours at 97 ℃.
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CN101838359A (en) * 2010-05-21 2010-09-22 上海宇昂生物科技有限公司 Non-ionic N-vinyl butyrate lactam iodine, high-stability non-ionic N-vinyl butyrate lactam iodine and relevant overspeed preparation method
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