CN105440965A - Preparation method of water-based nitrocellulose adhesive film - Google Patents
Preparation method of water-based nitrocellulose adhesive film Download PDFInfo
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- CN105440965A CN105440965A CN201510869170.8A CN201510869170A CN105440965A CN 105440965 A CN105440965 A CN 105440965A CN 201510869170 A CN201510869170 A CN 201510869170A CN 105440965 A CN105440965 A CN 105440965A
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Abstract
The invention discloses a preparation method of a water-based nitrocellulose adhesive film. The preparation method comprises the following steps: 1) weighing 1,5-diamino-3-sodium pentanesulfonate, butanone and recrystallized azodiisobutyronitrile, adding 1,5-diamino-3-sodium pentanesulfonate and butanone into a flask, adding the recrystallized azodiisobutyronitrile, adding dibutyltin dilaurate and isophorone diisocyanate into the flask under the protection of an inert gas, carrying out thermostatic stirring for reaction, rising the temperature, adding nitrocellulose dissolved with butanone, carrying out a heat-insulating reaction, lowering the temperature, adding deionized water while stirring is carried out, and carrying out heat-insulating dispersing to obtain a high-solid hydrous polymer emulsion; 2) adding the high-solid hydrous polymer emulsion obtained in the step 1) into a polytetrafluoroethylene board, forming a film via tape casting, putting the polytetrafluoroethylene board at a room temperature, and drying the polytetrafluoroethylene board to obtain the water-based nitrocellulose adhesive film. The water-based nitrocellulose adhesive film prepared according to the preparation method is relatively high in waterproofness and flexibility.
Description
Technical field
The present invention relates to a kind of preparation method of glued membrane, be specifically related to a kind of preparation method of aqueous nitrocellulose glued membrane.
Background technology
Nitrocotton (NC) has another name called nitro-cotton, is a kind of matrix of cellulose family tackiness agent.Traditional NC tackiness agent is all using organic solvent as dispersion medium, and it is in use easy in environment, and works the mischief to HUMAN HEALTH.
Aqueous nitrocellulose (WNC) emulsion is a kind of is dispersion medium with water, by introducing the stable NC aqueous dispersion made in hydrophilic radical to NC molecule.Compared with traditional solvent-borne NC tackiness agent, WNC emulsion has that VOC (volatile organic matter) content is almost 0, environmental protection little to harm and the advantage such as to economize on resources, and thus receives the concern of people gradually; But WNC emulsion is not good enough, the glued membrane water tolerance of existence and stability and the shortcoming such as snappiness is poor still.Therefore, for improving the application performance of WNC, modification must be carried out to improve water tolerance and the snappiness of WNC glued membrane to it.
Summary of the invention
The object of the invention is to the shortcoming overcoming above-mentioned prior art, a kind of preparation method of aqueous nitrocellulose glued membrane be provided, aqueous nitrocellulose glued membrane water tolerance prepared by the method and snappiness better.
For achieving the above object, for achieving the above object, the preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of rare gas element, dibutyl tin laurate and isophorone diisocyanate is added in flask, and 70-90 DEG C is warming up to after constant temperature stirring reaction under the condition of 60-70 DEG C, and then add butanone dissolve nitrocotton after insulation reaction, be cooled to 30-60 DEG C again, and add deionized water while stirring, be incubated dispersion again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 1-5g:10-20g:0.3-2g:0.1-0.8g:0.5-5.0g:2.0-5.0g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, then carries out drying again after at room temperature being placed by polyfluortetraethylene plate, obtains aqueous nitrocellulose glued membrane.
Step 1) in flask, add dibutyl tin laurate and isophorone diisocyanate, and be warming up to 70-90 DEG C after 500rpm constant temperature stirring reaction 15min with speed at the temperature of 60-70 DEG C.
Described rare gas element is nitrogen.
Step 1) in add insulation reaction 2h after the nitrocotton that butanone dissolves, then be cooled to 30-60 DEG C, and limit is stirred limit with 3000rpm speed and is added deionized water.
Step 1) in insulation dispersion time be 30min.
The thickness of described aqueous nitrocellulose glued membrane is 1mm.
Step 1) in flask, add the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate.
Step 2) concrete operations be: by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane.
The present invention has following beneficial effect:
The preparation method of aqueous nitrocellulose glued membrane of the present invention is in the process preparing aqueous nitrocellulose glued membrane, with the Diisopropyl azodicarboxylate initiator of recrystallization, by 1,5-diamino-3-penta sodium sulfonate by the hydrophilic group of a greater number because being incorporated in macromolecular chain, thus prepare large arch dam aqueous high molecular emulsion, again by dry after described large arch dam aqueous high molecular emulsion casting film-forming, obtain aqueous nitrocellulose glued membrane, aqueous nitrocellulose glued membrane dispersiveness, water tolerance and snappiness that the present invention prepares are better, and film forming speed is very fast.
Embodiment
Being described in further detail the present invention below in conjunction with specific embodiment, is below explanation of the invention instead of restriction.
Embodiment one
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 70 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 60 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 30 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 1g:20g:0.3g:0.8g:0.5g:5.0g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
Embodiment two
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 90 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 70 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 60 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 5g:10g:2g:0.1g:5.0g:2.0g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
Embodiment three
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 80 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 65 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 45 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 3g:15g:1g:0.5g:3g:3.5g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
Embodiment four
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 75 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 63 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 35 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 2g:13g:0.8g:0.3g:2g:2.5g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
Embodiment five
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 85 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 68 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 50 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 4g:18g:1.8g:0.6g:4g:4g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
Embodiment six
The preparation method of aqueous nitrocellulose glued membrane of the present invention comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of nitrogen, the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate is added in flask, and be warming up to 76 DEG C after 500rpm constant temperature stirring reaction 15min with speed under the condition of 66 DEG C, and then add butanone dissolve nitrocotton after insulation reaction 2h, be cooled to 48 DEG C again, and limit adds deionized water with 3000rpm speed stirring limit, insulation dispersion 30min again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 2.8g:13g:1.1g:0.2g:1.6g:2.7g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, polyfluortetraethylene plate is taken out, after its cooling, obtain aqueous nitrocellulose glued membrane, wherein, the thickness of aqueous nitrocellulose glued membrane is 1mm.
The contact angle recording aqueous nitrocellulose glued membrane is 105.15 °, is greater than 90 ° and has good water tolerance.(20 DEG C) under large arch dam aqueous high molecular emulsion room temperature are placed 90 days, has no the phenomenon such as layering, coagulation; With whizzer centrifugal for emulsion two hours, leave standstill and have no layering; Place 12 hours in refrigerated tank, take out room temperature and place 12 hours, 5 times so repeatedly, have no layering, freeze the phenomenons such as caking.
Claims (8)
1. a preparation method for aqueous nitrocellulose glued membrane, is characterized in that, comprises the following steps:
1) 1 is taken, 5-diamino-3-penta sodium sulfonate, the Diisopropyl azodicarboxylate of butanone and recrystallization, by 1, 5-diamino-3-penta sodium sulfonate and butanone join in flask, add the Diisopropyl azodicarboxylate of recrystallization again, and under the protection of rare gas element, dibutyl tin laurate and isophorone diisocyanate is added in flask, and 70-90 DEG C is warming up to after constant temperature stirring reaction under the condition of 60-70 DEG C, and then add butanone dissolve nitrocotton after insulation reaction, be cooled to 30-60 DEG C again, and add deionized water while stirring, be incubated dispersion again, obtain large arch dam aqueous high molecular emulsion, wherein, the ratio of the Diisopropyl azodicarboxylate of 1,5-diamino-3-penta sodium sulfonate, butanone, recrystallization, dibutyl tin laurate, isophorone diisocyanate, nitrocotton and deionized water is: 1-5g:10-20g:0.3-2g:0.1-0.8g:0.5-5.0g:2.0-5.0g:40ml,
2) by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, then carries out drying again after at room temperature being placed by polyfluortetraethylene plate, obtains aqueous nitrocellulose glued membrane.
2. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, it is characterized in that, step 1) in flask, add dibutyl tin laurate and isophorone diisocyanate, and be warming up to 70-90 DEG C after 500rpm constant temperature stirring reaction 15min with speed at the temperature of 60-70 DEG C.
3. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, is characterized in that, described rare gas element is nitrogen.
4. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, is characterized in that, step 1) in add insulation reaction 2h after the nitrocotton that butanone dissolves, then be cooled to 30-60 DEG C, and limit is stirred limit with 3000rpm speed and is added deionized water.
5. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, is characterized in that, step 1) in insulation dispersion time be 30min.
6. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, is characterized in that, the thickness of described aqueous nitrocellulose glued membrane is 1mm.
7. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, is characterized in that, step 1) in flask, add the dibutyl tin laurate after the process of 4A molecular sieve dehydration and isophorone diisocyanate.
8. the preparation method of aqueous nitrocellulose glued membrane according to claim 1, it is characterized in that, step 2) concrete operations be: by step 1) the large arch dam aqueous high molecular emulsion that obtains pours casting film-forming in polyfluortetraethylene plate into, drying oven is put into again after again polyfluortetraethylene plate at room temperature being placed 24h, and in drying oven under the condition of 40 DEG C dry 24h, then from drying oven, take out polyfluortetraethylene plate, after its cooling, obtain aqueous nitrocellulose glued membrane.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101437484A (en) * | 2006-04-07 | 2009-05-20 | 拜尔材料科学股份公司 | Nitrocellulose-based binders for aqueous nail polishes |
| CN103819710A (en) * | 2014-03-04 | 2014-05-28 | 苏州奥特福环境科技有限公司 | Method for preparing hydrophilic nitrated cellulose film |
| CN104479137A (en) * | 2014-12-03 | 2015-04-01 | 陕西科技大学 | Preparation method of water-based nitrocellulose emulsion and nitrocellulose film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101437484A (en) * | 2006-04-07 | 2009-05-20 | 拜尔材料科学股份公司 | Nitrocellulose-based binders for aqueous nail polishes |
| CN103819710A (en) * | 2014-03-04 | 2014-05-28 | 苏州奥特福环境科技有限公司 | Method for preparing hydrophilic nitrated cellulose film |
| CN104479137A (en) * | 2014-12-03 | 2015-04-01 | 陕西科技大学 | Preparation method of water-based nitrocellulose emulsion and nitrocellulose film |
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