CN103450385B - A kind of preparation method of high-molecular humidity-controlling agent that can highly effective humidity conditioning - Google Patents
A kind of preparation method of high-molecular humidity-controlling agent that can highly effective humidity conditioning Download PDFInfo
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Abstract
The present invention discloses a kind of preparation method of high-molecular humidity-controlling agent that can highly effective humidity conditioning. Acrylic acid adds and in NaOH solution, obtains adjusting the acrylic acid solution after pH value; Add again methacrylic acid, acrylamide, after mixing, obtain mixed solution; Be placed in warm water and fill nitrogen deoxygenation 0.5～2 hour, then add crosslinking agent, initator, form reaction solution; Be placed in 50～70 DEG C of waters bath with thermostatic control and heat, react 3～6 hours, obtain gel polymerizate, finally section, granulation, drying and processing, pulverize, sieve, obtain final products. Adopt the high-molecular humidity-controlling agent prepared of the method have damping capacity greatly, the advantage such as the low and renewable use of responding ability, cost fast, and this preparation method have molecular weight of product relatively evenly, technique is simple, cost is low and be easy to the advantages such as control, be easy to realize industrialized feature.
Description
Technical field
The invention belongs to environmental-friendly construction material field, be specifically related to a kind of preparation method of high-molecular humidity-controlling agent that can highly effective humidity conditioning.
Background technology
South China rainfall is many, continues a day cloudy rainy plum rain season between especially annual first half of the month in mid or late June to July, and air humidity is large, temperature is high, and clothing etc. are easily mouldy. For example, mostly modern construction house is the materials such as panelling, prefabricated board (or top goods), armored concrete, metal slide window, therefore air-tightness is high, the problem of dewfall is many. Its reason is that house air-tightness is good, ventilates poor, and living standard improves, and water increases, and uses the greenhouse utensils such as petroleum gas stove, gas burner etc., causes dewfall to see and resembles seriously. Particularly the moist house such as kitchen, bathhouse, washing room, large-scale indoor publilc baths is serious especially in the dewfall on wall, roof, ground.
Humidity adjusting material refers to need to be by any artificial energy source and plant equipment, relies on the humidity of the moisture adsorption and releasing characteristic induction space air of adjusting of self to change, and automatically regulates the functional material of humidity. In the time that humidity is higher, humidity adjusting material can adsorb the steam in environment, and the humidity in space is reduced; In the time that humidity is lower, material will discharge the steam self adsorbing, and increases the relative humidity in space, thereby keeps the relatively constant of environment space humidity. The wallpaper that has for example added conditioning agent can anti-condensation, regulates the humidity in room; Additive and conditioning agent are mixed with to humidity controlling coating, for the inwall of building, the top finishing of storage facilities inwall, thereby reach the object of damping; By rubber and high-molecular humidity-controlling agent and with making sealing (water proof) material, be commonly used in the civil construction project field such as airtight, waterproof of filling, sealing, sealing and all kinds of machines of building construction gap.
Utilize the moisture adsorption and releasing characteristic of humidity adjusting material to regulate humidity, although be a kind of passive control measure, it is without any plant equipment and energy resource consumption, because of but a kind of control and regulation method of ecological property. This for improve human settlement, plant (flowers, crops etc.) healthy growth, improve preservation quality, the instrument of article (food, medicine, historical relic) normal operation, maintain the sustainable development of ecological environment, all there is undoubtedly important using value and social effect.
Summary of the invention
The object of the present invention is to provide that a kind of technique is simple, with low cost, energy resource consumption is low and the preparation method of the high-molecular humidity-controlling agent of highly effective humidity conditioning, make it to be suitable for dehumidification system, sealing (water proof) material and humidity controlling coating etc. and need to regulate the occasion of humidity.
The inventive method comprises the following steps:
Step (1). acrylic acid is joined in the reactor that agitator is housed, adding while stirring concentration is the NaOH solution of 14～20 ﹪, obtains acrylic acid solution;
Wherein, the quality of NaOH=(acrylic acid+methacrylic acid) × (65 ﹪～85 ﹪) × 40, acrylic acid and methacrylic acid are amount of substance, and unit is mol, 40 molecular weight that are NaOH, 65 ﹪～85 ﹪ are degree of neutralization.
Step (1) is carried out in ice-water bath, prevents that sodium hydroxide solution heating from can cause acrylic acid volatilization.
Step (2). in the acrylic acid solution of adjusting after pH value, add while stirring methacrylic acid, acrylamide, after mixing, obtain mixed solution; Wherein, the mass ratio of methacrylic acid, acrylic acid, acrylamide is (2～18): (1～3): 1;
Step (3). by the mixed solution of step (2) preparation, the warm water that is placed in temperature and is 22～25 DEG C fills nitrogen deoxygenation 0.5～2 hour, then adds crosslinking agent, initator, after stirring, finally forms reaction solution.
Wherein, the quality of crosslinking agent=(acrylic acid+acrylamide+methacrylic acid) × (0.2 ﹪～2 ﹪), wherein acrylic acid, acrylamide and methacrylic acid are quality, and unit is g; Quality=(acrylic acid+acrylamide+methacrylic acid) × (0.2 ﹪～2 ﹪) of initator, wherein acrylic acid, acrylamide and methacrylic acid are quality, and unit is g.
Described crosslinking agent is N hydroxymethyl acrylamide, N, N '-methylene-bisacrylamide or DAAM;
Described initator is potassium peroxydisulfate, sodium hydrogensulfite/ammonium persulfate, hydrogen peroxide, ammonium persulfate/ferrous sulfate or sodium peroxydisulfate;
Step (4). it is that the water bath with thermostatic control of 50～70 DEG C is heated that the reaction solution that step (3) is obtained is placed in temperature, allows it fully react 3～6 hours, obtains gel polymerizate.
Step (5). the gel polymerizate that step (4) is obtained through section, granulation, drying and processing, pulverize, sieve after, obtain prepared by the present invention can highly effective humidity conditioning high-molecular humidity-controlling agent.
The thickness of described gel polymerizate after section is 0.5～1.5cm;
Described drying and processing is to dry 4～6 hours at 80～120 DEG C of temperature, does not change to the quality of gel polymerizate;
45～60 orders are selected in described sieving.
It is monomer that the present invention adopts acrylic acid, acrylamide and methacrylic acid etc., by the mutual synergy of the multiple group such as hydroxy-acid group, amide group in copolymer, improve significantly the humidity of high-molecular humidity-controlling agent, and the applicable different occasion of the shape of product variation. Compare mineral-type humidity adjusting material, tool of the present invention has the following advantages:
1. in the mineral-type such as silica gel and molecular sieve conditioning agent dozens of minutes, just reach moisture absorption saturated, no longer play a role; And this high-molecular humidity-controlling agent does not reach after 7 days that moisture absorption is saturated and damping capacity is large yet, the highest hygroscopic capacity can reach 0.95g/g, has embodied the superiority of long-acting damping.
2. preparation technology is simple, adopts " one kettle way " to realize.
3. regeneration energy consumption is low, and the humidity after regeneration declines and is no more than 2 ﹪.
Adopt the high-molecular humidity-controlling agent prepared of the method have damping capacity greatly, the advantage such as the low and renewable use of responding ability, cost fast, be widely used in anti-condensation and damping wallpaper, dewfall and prevent the industry such as sheet and humidity-regulating sheet, humidity controlling coating, water proof material and building. And this preparation method has, and molecular weight of product is relatively more even, technique is simple, cost is low and be easy to the advantages such as control, be easy to realize industrialized feature.
Detailed description of the invention
Specific embodiments of the invention are described as follows, but the scope that also unrestricted the present invention explains is only for more specifically illustrating feature of the present invention.
Embodiment 1
(1) get 3g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 18.3 ﹪, obtains acrylic acid solution. Wherein, in NaOH solution, the quality of NaOH is 19.1g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization.
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 54g methacrylic acid, 3g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 25 DEG C of warm water fills nitrogen deoxygenation 0.5 hour, adds afterwards 0.18gN-NMA and 0.18g potassium peroxydisulfate, the final reaction solution that forms after fully stirring.
(5) the reaction solution that (4) step prepares is heated in the water bath with thermostatic control of 65 DEG C, allow it fully react 3 hours, obtain gel polymerizate.
By the product that (5) step obtains at section, granulation, 120 DEG C drying and processing 4h, pulverize, sieve, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 1 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Finally recording its hygroscopic capacity is 0.825g/g.
Regenerability: high-molecular humidity-controlling agent regeneration prepared embodiment 1 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
Embodiment 2
(1) get 15g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 16 ﹪, obtains acrylic acid solution. Wherein, in NaOH solution, the quality of NaOH is 16.7g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization.
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 30g methacrylic acid, 15g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 25 DEG C of warm water fills nitrogen deoxygenation 0.7 hour, adds afterwards 0.18gN, N '-methylene-bisacrylamide and 0.18g sodium hydrogensulfite/ammonium persulfate, the final reaction solution that forms after fully stirring.
(5) the mixed solution that (4) step prepares is heated in the water bath with thermostatic control of 65 DEG C, allow it fully react 3 hours, obtain gel polymerizate.
By the product that (5) step obtains through drying and processing 4h at section, granulation, 120 DEG C, pulverize, sieve after, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 2 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Finally recording its hygroscopic capacity is 0.885g/g.
The prepared high-molecular humidity-controlling agent regeneration of regenerability: embodiment 2 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
Embodiment 3
(1) get 5.5g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 14 ﹪, obtains mixed solution. Wherein, in NaOH solution, the quality of NaOH is 10.21g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization;
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 19.25g methacrylic acid, 2.75g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 25 DEG C of warm water fills nitrogen deoxygenation 0.5 hour, adds afterwards 0.25g DAAM and 0.35g hydrogen peroxide, the final reaction solution that forms after fully stirring.
(5) the reaction solution that (4) step prepares is heated in the water bath with thermostatic control of 65 DEG C, allow it fully react 4 hours, obtain gel polymerizate.
By the product that (5) step obtains through drying and processing 4h at section, granulation, 120 DEG C, pulverize, sieve after, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 3 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Its hygroscopic capacity is 0.95g/g.
Regenerability: high-molecular humidity-controlling agent regeneration prepared embodiment 3 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
Embodiment 4
(1) get 6.5g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 14.2 ﹪, obtains acrylic acid solution. Wherein, in NaOH solution, the quality of NaOH is 9.52g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization.
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 19.5g methacrylic acid, 6.5g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 25 DEG C of warm water fills nitrogen deoxygenation 0.5 hour, adds afterwards 0.2gN-NMA, 0.4g ammonium persulfate/ferrous sulfate, the final mixed solution that forms after fully stirring.
(5) the mixed solution that (4) step prepares is heated in the water bath with thermostatic control of 65 DEG C, allow it fully react 3 hours, obtain gel polymerizate.
By the product that (5) step obtains through drying and processing 4h at section, granulation, 120 DEG C, pulverize, sieve after, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 4 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Its hygroscopic capacity is 0.87g/g.
Regenerability: high-molecular humidity-controlling agent regeneration prepared embodiment 4 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
Embodiment 5
(1) get 15g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 20 ﹪, obtains acrylic acid solution. Wherein, in NaOH solution, the quality of NaOH is 14.5g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization.
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 30g methacrylic acid, 5g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 22 DEG C of warm water fills nitrogen deoxygenation 2 hours, adds afterwards 0.1gN, N '-methylene-bisacrylamide, 0.1g sodium peroxydisulfate, the final mixed solution that forms after fully stirring.
(5) the mixed solution that (4) step prepares is heated in the water bath with thermostatic control of 50 DEG C, allow it fully react 6 hours, obtain gel polymerizate.
By the product that (5) step obtains through drying and processing 6h at section, granulation, 80 DEG C, pulverize, sieve after, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 5 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Its hygroscopic capacity is 0.88g/g.
Regenerability: high-molecular humidity-controlling agent regeneration prepared embodiment 5 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
Embodiment 6
(1) get 6g acrylic acid and join in the there-necked flask that agitator is housed, adding while stirring concentration is the NaOH solution of 15 ﹪, obtains acrylic acid solution. Wherein, in NaOH solution, the quality of NaOH is 9.17g.
(2) (1) walk and carry out in ice-water bath, prevent that sodium hydroxide solution heating from can cause acrylic acid volatilization.
(3) by the acrylic acid solution that (1) walks modulated good pH value, add while stirring 21g methacrylic acid, 3g acrylamide, obtain mixed solution.
(4) by the mixed solution that (3) step prepares, being placed in 22 DEG C of warm water fills nitrogen deoxygenation 1.5 hours, adds afterwards 0.6g DAAM, 0.6g potassium peroxydisulfate, the final mixed solution that forms after fully stirring.
(5) the mixed solution that (4) step prepares is heated in the water bath with thermostatic control of 70 DEG C, allow it fully react 3 hours, obtain gel polymerizate.
By the product that (5) step obtains through drying and processing 5h at section, granulation, 100 DEG C, pulverize, sieve after, obtain the high-molecular humidity-controlling agent of highly effective humidity conditioning.
(7) performance test:
Moisture pick-up properties: high-molecular humidity-controlling agent prepared embodiment 6 is put into climatic chamber and carry out moisture absorption, until moisture absorption is saturated. Test condition is: T=25 DEG C, RH=90 ﹪. Its hygroscopic capacity is 0.90g/g.
Regenerability: high-molecular humidity-controlling agent regeneration prepared embodiment 6 is processed, and the balance Moisture absorption rate of regenerating after five times declines and is also no more than 2 ﹪.
The thickness that (6) above-described embodiment the walks the gel polymerizate after section is 0.5～1.5cm; Sieve and select 45～60 orders.
Above-described embodiment is not that the present invention is not limited only to above-described embodiment for restriction of the present invention, as long as meet requirement of the present invention, all belongs to protection scope of the present invention.
Claims (5)
1. a preparation method for high-molecular humidity-controlling agent that can highly effective humidity conditioning, is characterized in that the method comprises the following steps:
Step (1). acrylic acid is joined in the reactor that agitator is housed, adding while stirring concentration is the NaOH solution of 14～20 ﹪, obtains acrylic acid solution;
Wherein, the quality of NaOH=(acrylic acid+methacrylic acid) × (65 ﹪～85 ﹪) × 40; Acrylic acid and methacrylic acid are amount of substance, and unit is mol; 40 is the molecular weight of NaOH; 65 ﹪～85 ﹪ are degree of neutralization;
Step (2). in the acrylic acid solution after adjust pH, add while stirring methacrylic acid, acrylamide, after mixing, obtain mixed solution; Wherein the mass ratio of methacrylic acid, acrylic acid, acrylamide is 18:1:1,2:1:1,3:1:1,6:3:1 or 7:2:1;
Step (3). by the mixed solution of step (2) preparation, the warm water that is placed in temperature and is 22～25 DEG C fills nitrogen deoxygenation 0.5～2 hour, then adds crosslinking agent, initator, after stirring, finally forms reaction solution;
Wherein, the quality of crosslinking agent=(acrylic acid+acrylamide+methacrylic acid) × (0.2 ﹪～2 ﹪), wherein acrylic acid, acrylamide and methacrylic acid are quality, and unit is g; Quality=(acrylic acid+acrylamide+methacrylic acid) × (0.2 ﹪～2 ﹪) of initator, wherein acrylic acid, acrylamide and methacrylic acid are quality, and unit is g;
Step (4). it is that the water bath with thermostatic control of 50～70 DEG C is heated that the reaction solution that step (3) is obtained is placed in temperature, allows it fully react 3～6 hours, obtains gel polymerizate;
Step (5). the gel polymerizate that step (4) is obtained through section, granulation, drying and processing, pulverize, sieve after, obtain can highly effective humidity conditioning high-molecular humidity-controlling agent;
Described crosslinking agent is N hydroxymethyl acrylamide or DAAM;
Described initator is hydrogen peroxide, ammonium persulfate/ferrous sulfate or sodium peroxydisulfate.
2. the preparation method of a kind of high-molecular humidity-controlling agent that can highly effective humidity conditioning as claimed in claim 1, is characterized in that step (1) carries out in ice-water bath, prevents that sodium hydroxide solution heating from can cause acrylic acid volatilization.
3. the preparation method of a kind of high-molecular humidity-controlling agent that can highly effective humidity conditioning as claimed in claim 1, is characterized in that the thickness of the gel polymerizate of step (5) after section is 0.5～1.5cm.
4. the preparation method of a kind of high-molecular humidity-controlling agent that can highly effective humidity conditioning as claimed in claim 1, it is characterized in that the described drying and processing of step (5) is to dry 4～6 hours at 80～120 DEG C of temperature, do not change to the quality of gel polymerizate.
5. the preparation method of a kind of high-molecular humidity-controlling agent that can highly effective humidity conditioning as claimed in claim 1, is characterized in that described the sieving of step (5) select 45～60 orders.
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| CN101225139A (en) * | 2007-12-21 | 2008-07-23 | 中国科学院长春应用化学研究所 | Method for preparing polyacrylic acid/acrylamide moisture-absorption resin |
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| JPH1081714A (en) * | 1996-09-04 | 1998-03-31 | Toagosei Co Ltd | Water absorbing resin |
| CN101225138A (en) * | 2007-12-20 | 2008-07-23 | 中国科学院长春应用化学研究所 | Method for preparing polymethacrylic acid moisture-absorption resin |
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| 聚丙烯酸-甲基丙烯酸-丙烯酰胺P(AA-MA-AM)三元共聚物的合成及其吸湿性能研究;张春晓等;《功能材料》;20111231;第42卷;282-286 * |
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Effective date of registration: 20170112 Address after: 310000 Yuhang economic and Technological Development Zone, Yuhang District, Hangzhou Chao Feng Road, No., building No. 1, building 146 Patentee after: ZHEJIANG HAICHUANG MEDICAL DEVICE CO., LTD. Address before: Hangzhou City, Zhejiang province 310018 Xiasha Higher Education Park No. 2 street Patentee before: Hangzhou Electronic Science & Technology Univ. |