CN103145906A - Preparation method of environment-friendly type core-shell propyl acetate emulsion - Google Patents
Preparation method of environment-friendly type core-shell propyl acetate emulsion Download PDFInfo
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- CN103145906A CN103145906A CN2013100276869A CN201310027686A CN103145906A CN 103145906 A CN103145906 A CN 103145906A CN 2013100276869 A CN2013100276869 A CN 2013100276869A CN 201310027686 A CN201310027686 A CN 201310027686A CN 103145906 A CN103145906 A CN 103145906A
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Abstract
The invention provides a preparation method of environment-friendly type core-shell propyl acetate emulsion. The preparation method includes the following steps of preparing the core of the emulsion, and then preparing a shell of the emulsion through an in-situ polymerization, wherein used emulgator without alkylphenol ethoxylates (APEO) and crosslink monomer without formaldehyde are all of an environment-friendly type. Compared with the prior art, the preparation method of the environment-friendly type core-shell propyl acetate emulsion is convenient to operate, the finally prepared emulsion is even in particle size distribution, low in film formation temperature, and good in water resistance, heat resistance, ageing resistance and freeze thawing stability.
Description
Technical field
The present invention relates to a kind of adhesive technology field, specifically a kind of preparation method of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion.
Background technology
In recent years, along with improving constantly of people's environmental consciousness, people had also proposed stricter condition to the use of the starting material in water-base resin, water-borne coatings and auxiliary agent.Mostly can discharge formaldehyde and mostly contain in traditional nonionic emulsifying agent in APEO, traditional linking agent, therefore in order to prepare the water-based emulsion that meets following environmental requirement, just need to use the starting material of the environment-friendly type of series of new.
Acrylate and vinyl acetate emulsion has its natural special advantage, and is as lower in cost, flow leveling is good, lacquering has texture.But shortcoming is also comparatively obvious, and such as poor water resistance, resistance to elevated temperatures is poor, not anti-xanthochromia.Therefore how preparing high performance acrylate and vinyl acetate emulsion is also the direction that many technical staff authors study for many years.And hud typed acrylate and vinyl acetate emulsion has special technique and preparation method due to it, by preparing respectively stratum nucleare and shell, has just made up a lot of shortcomings of acrylate and vinyl acetate emulsion.Make it have significant performance to improve aspect water-fast, heat-resisting, ageing-resistant.Especially with the interiro wall latex paint of this kind method preparation, has excellent water tolerance, scrub performance, and toning excellent performance.
In the nucleocapsid acrylate and vinyl acetate emulsion making processes of prior art, the feature of environmental protection is relatively poor, has very large deficiency, for making up this deficiency, the invention provides a kind of preparation method of nucleocapsid acrylate and vinyl acetate emulsion of environmental protection.
Summary of the invention
Technical assignment of the present invention is to solve the deficiencies in the prior art, and the preparation method of the environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion that a kind of emulsion particle diameter of preparing is evenly distributed and film-forming temperature is low is provided.
Technical scheme of the present invention realizes in the following manner, the preparation method of this a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion, and its concrete preparation process is:
1) will stir after 100～150 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, 0～50 part, vinylformic acid, nonionic emulsifying agent EH-400.5～1 part, 0.1～0.5 part of Sodium dodecylbenzene sulfonate, 700～800 parts of mixing of deionized water, be heated to after certain temperature ascorbic acid solution with the hydrogen peroxide solution of 20～50 parts and 20～50 parts and drip simultaneously and enter in mixing solutions, make stratum nucleare structure seed emulsion standby;
10～30 parts of 300～450 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, vinylformic acid are mixed with into shell monomers standby;
1～3 part of Potassium Persulphate, 50～80 parts of deionized water solutions are carried out fully dissolving, and to make initiator solution standby;
2) will stir and be heated to certain temperature after 0.5～1 part of Mierocrystalline cellulose, nonionic emulsifying agent EH-400.2～2 part, 0.2～1 part of Sodium dodecylbenzene sulfonate, 1～2 part, sodium bicarbonate and 400～500 parts of mixing of deionized water;
3) wait reaching step 2) in after assigned temperature, add step 1) in the stratum nucleare structure seed emulsion of preparation;
4) add shell monomers and initiator solution after 5～10 minutes, adition process keeps constant temperature;
5) lower the temperature and regulate the pH value, filtering at last blowing.
Described step 1) in, preparation stratum nucleare structure seed emulsion acrylic ester monomer used refers to the one or more combination in butyl acrylate, Isooctyl acrylate monomer, ethyl propenoate; Preparation shell monomers esters of acrylic acid used is the one or more combination in ethyl propenoate, methyl methacrylate, tertiary ethylene carbonate.
Also add 3～8 parts of linking agent isobutoxy Methacrylamides when described step 1), stratum nucleare structure seed emulsion prepares, adding this linking agent is before heating.
Described step 1) Heating temperature is 68～75 ℃.
Described step 1) linking agent that in, stratum nucleare structure seed emulsion adds is 5 parts, and the hydrogen peroxide solution that adds is 3 parts, and the ascorbic acid solution that adds is 3 parts.
Described step 2) Heating temperature in is 75～80 ℃.
Described step 4) add the detailed step of shell monomers and initiator solution to be in: until step 3) dripped simultaneously step 3 in 5 minutes after completing) shell monomers and step 4) initiator solution, evenly drip 3 hours, the dropping process maintains the temperature at 80～83 ℃, dropwises rear insulation 1 hour.
Described step 5) cooling temperature is 40～50 ℃, and the pH value of adjusting is 5～6.
The beneficial effect that the present invention compared with prior art produces is:
The preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion of the present invention first prepares the core of emulsion, method by in-situ polymerization prepares shell again, and in preparation process, the emulsifying agent that does not contain APEO that uses and do not contain the cross-linking monomer of formaldehyde, this bi-material is all environment-friendly type, the emulsion particle diameter of preparing at last be evenly distributed and film-forming temperature low, have excellent water tolerance, thermotolerance, ageing resistance and freeze-thaw stability.
Embodiment
The below is described in detail below the preparation method of this a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion to the preparation method to a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion of the present invention, its concrete preparation process is:
1) will stir after 100～150 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, 0～50 part, vinylformic acid, nonionic emulsifying agent EH-400.5～1 part, 0.1～0.5 part of Sodium dodecylbenzene sulfonate, 700～800 parts of mixing of deionized water, be heated to after certain temperature ascorbic acid solution with the hydrogen peroxide solution of 20～50 parts and 20～50 parts and drip simultaneously and enter in mixing solutions, make stratum nucleare structure seed emulsion standby;
10～30 parts of 300～450 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, vinylformic acid are mixed with into shell monomers standby;
1～3 part of Potassium Persulphate, 50～80 parts of deionized water solutions are carried out fully dissolving, and to make initiator solution standby;
2) will stir and be heated to certain temperature after 0.5～1 part of Mierocrystalline cellulose, nonionic emulsifying agent EH-400.2～2 part, 0.2～1 part of Sodium dodecylbenzene sulfonate, 1～2 part, sodium bicarbonate and 400～500 parts of mixing of deionized water;
3) wait reaching step 2) in after assigned temperature, add step 1) in the stratum nucleare structure seed emulsion of preparation;
4) add shell monomers and initiator solution after 5～10 minutes, adition process keeps constant temperature;
5) lower the temperature and regulate the pH value, filtering at last blowing.
Described step 1) in, preparation stratum nucleare structure seed emulsion acrylic ester monomer used refers to the one or more combination in butyl acrylate, Isooctyl acrylate monomer, ethyl propenoate; Preparation shell monomers esters of acrylic acid used is the one or more combination in ethyl propenoate, methyl methacrylate, tertiary ethylene carbonate.
Also add 3～8 parts of linking agent isobutoxy Methacrylamides when described step 1), stratum nucleare structure seed emulsion prepares, adding this linking agent is before heating.
Described step 1) Heating temperature is 68～75 ℃.
Described step 1) linking agent that in, stratum nucleare structure seed emulsion adds is 5 parts, and the hydrogen peroxide solution that adds is 3 parts, and the ascorbic acid solution that adds is 3 parts.
Described step 2) Heating temperature in is 75～80 ℃.
Described step 4) add the detailed step of shell monomers and initiator solution to be in: until step 3) dripped simultaneously step 3 in 5 minutes after completing) shell monomers and step 4) initiator solution, evenly drip 3 hours, the dropping process maintains the temperature at 80～83 ℃, dropwises rear insulation 1 hour.
Described step 5) cooling temperature is 40～50 ℃, and the pH value of adjusting is 5～6.
Example 1: EH-40, the 0.2g Sodium dodecylbenzene sulfonate of 750g deionized water, 0.8g are dropped in four-hole boiling flask, and then drop into successively vinyl acetate 100g, butyl acrylate 80g, vinylformic acid 20g.Start and stir and heating in water bath to 70 ℃.Drip simultaneously 1% hydrogen peroxide solution 30g and 1% ascorbic acid solution 30g this moment, and time for adding is 20 minutes.Dropwise rear insulation and emit the stratum nucleare seed emulsion after 20 minutes.
EH-40,0.5g Sodium dodecylbenzene sulfonate, the 1g sodium bicarbonate of 500g deionized water, 1g Mierocrystalline cellulose QP-300,1g are dropped in four-hole boiling flask, start and stir and be heated to 80 ℃.Then add stratum nucleare structure seed emulsion 100g.
300g Vinyl Acetate Monomer, 80g methyl methacrylate, 20g vinylformic acid are carried out fully mixing form shell monomers.2g Potassium Persulphate and 60g water fully are mixed into initiator solution.
Drip simultaneously shell monomers and initiator solution in the time of 80 ℃.Time for adding is 3.5 hours.In the dropping process, temperature is controlled to be 80-82 ℃.Drip and finish rear insulation 1 hour.Be cooled to 45 ℃ after insulation finishes and neutralize, filter blowing with ammonia neutralization to 5-6.
Example 2: EH-40, the 0.5g Sodium dodecylbenzene sulfonate of 700g deionized water, 0.5g are dropped in four-hole boiling flask, and then drop into successively vinyl acetate 120g, Isooctyl acrylate monomer 60g, vinylformic acid 15g, 5g cross-linking monomer IBMA (isobutoxy Methacrylamide).Start and stir and heating in water bath to 70 ℃.Drip simultaneously 1% hydrogen peroxide solution 30g and 1% ascorbic acid solution 30g this moment, and time for adding is 20 minutes.Dropwise rear insulation and emit the stratum nucleare seed emulsion after 20 minutes.
EH-40,1g Sodium dodecylbenzene sulfonate, the 2g sodium bicarbonate of 450g deionized water, 0.5g Mierocrystalline cellulose QP-300,2g are dropped in four-hole boiling flask, start and stir and be heated to 80 ℃.Then add stratum nucleare structure seed emulsion 120g.
400g Vinyl Acetate Monomer, 50g tertiary ethylene carbonate, 30g vinylformic acid are carried out fully mixing form shell monomers.2g Potassium Persulphate and 60g water fully are mixed into initiator solution.
Drip simultaneously shell monomers and initiator solution in the time of 80 ℃.Time for adding is 3.5 hours.In the dropping process, temperature is controlled to be 80-82 ℃.Drip and finish rear insulation 1 hour.Be cooled to 45 ℃ after insulation finishes and neutralize, filter blowing with ammonia neutralization to 5-6.
Claims (8)
1. the preparation method of an environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion, it is characterized in that: its concrete preparation process is:
1) will stir after 100～150 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, 0～50 part, vinylformic acid, nonionic emulsifying agent EH-400.5～1 part, 0.1～0.5 part of Sodium dodecylbenzene sulfonate, 700～800 parts of mixing of deionized water, be heated to after certain temperature ascorbic acid solution with the hydrogen peroxide solution of 20～50 parts and 20～50 parts and drip simultaneously and enter in mixing solutions, make stratum nucleare structure seed emulsion standby;
10～30 parts of 300～450 parts of vinyl acetates, 50～100 parts of acrylic ester monomers, vinylformic acid are mixed with into shell monomers standby;
1～3 part of Potassium Persulphate, 50～80 parts of deionized water solutions are carried out fully dissolving, and to make initiator solution standby;
2) will stir and be heated to certain temperature after 0.5～1 part of Mierocrystalline cellulose, nonionic emulsifying agent EH-400.2～2 part, 0.2～1 part of Sodium dodecylbenzene sulfonate, 1～2 part, sodium bicarbonate and 400～500 parts of mixing of deionized water;
3) wait reaching step 2) in after assigned temperature, add step 1) in the stratum nucleare structure seed emulsion of preparation;
4) add shell monomers and initiator solution after 5～10 minutes, adition process keeps constant temperature;
5) lower the temperature and regulate the pH value, filtering at last blowing.
2. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 1 is characterized in that: described step 1), preparation stratum nucleare structure seed emulsion acrylic ester monomer used refers to the one or more combination in butyl acrylate, Isooctyl acrylate monomer, ethyl propenoate; Preparation shell monomers esters of acrylic acid used is the one or more combination in ethyl propenoate, methyl methacrylate, tertiary ethylene carbonate.
3. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 1, it is characterized in that: also add 3～8 parts of linking agent isobutoxy Methacrylamides when described step 1), stratum nucleare structure seed emulsion prepares, adding this linking agent is before heating.
4. the preparation method of according to claim 1 or 3 described a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsions, it is characterized in that: Heating temperature described step 1) is 68～75 ℃.
5. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 3, it is characterized in that: the linking agent that described step 1), stratum nucleare structure seed emulsion adds is 5 parts, the hydrogen peroxide solution that adds is 3 parts, and the ascorbic acid solution that adds is 3 parts.
6. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 1, it is characterized in that: the Heating temperature described step 2) is 75～80 ℃.
7. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 1, it is characterized in that described step 4) in add the detailed step of shell monomers and initiator solution to be: until step 3) dripped simultaneously step 3 in 5 minutes after completing) shell monomers and step 4) initiator solution, evenly drip 3 hours, the dropping process maintains the temperature at 80～83 ℃, dropwises rear insulation 1 hour.
8. the preparation method of a kind of environment-friendly type nucleocapsid acrylate and vinyl acetate emulsion according to claim 1, it is characterized in that: cooling temperature described step 5) is 40～50 ℃, the pH value of adjusting is 5～6.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952100A (en) * | 2013-10-12 | 2014-07-30 | 台州市顶立胶粘剂有限公司 | Environment-friendly adhesive for hot-fix rhinestone polishing processing of crystals and preparation method thereof |
| CN104231825A (en) * | 2014-09-19 | 2014-12-24 | 苏州云舒新材料科技有限公司 | Building interior wall latex and preparation method thereof |
| CN105418823A (en) * | 2016-01-19 | 2016-03-23 | 广东衡光化工有限公司 | High water-resistant and alkali-resistant and high scrub-resistant vinyl acetate-butyl acrylate emulsion as well as preparation of related coating |
| CN105482021A (en) * | 2016-01-19 | 2016-04-13 | 广东衡光化工有限公司 | Vac-veova emulsion with excellent comprehensive performance and preparation method of related coating |
| CN109824813A (en) * | 2018-12-12 | 2019-05-31 | 常熟巴德富科技有限公司 | A kind of acrylate and vinyl acetate emulsion and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730592A (en) * | 2005-09-14 | 2006-02-08 | 北京高盟化工有限公司 | Composite adhesive for soft wrapper and its preparation method |
-
2013
- 2013-01-25 CN CN2013100276869A patent/CN103145906A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1730592A (en) * | 2005-09-14 | 2006-02-08 | 北京高盟化工有限公司 | Composite adhesive for soft wrapper and its preparation method |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103952100A (en) * | 2013-10-12 | 2014-07-30 | 台州市顶立胶粘剂有限公司 | Environment-friendly adhesive for hot-fix rhinestone polishing processing of crystals and preparation method thereof |
| CN103952100B (en) * | 2013-10-12 | 2016-01-20 | 台州市顶立胶粘剂有限公司 | Environment-friendly adhesive for hot-fix rhinestone polishing processing of crystals and preparation method thereof |
| CN104231825A (en) * | 2014-09-19 | 2014-12-24 | 苏州云舒新材料科技有限公司 | Building interior wall latex and preparation method thereof |
| CN104231825B (en) * | 2014-09-19 | 2016-05-25 | 苏州云舒新材料科技有限公司 | A kind of inner wall of building latex and preparation method thereof |
| CN105418823A (en) * | 2016-01-19 | 2016-03-23 | 广东衡光化工有限公司 | High water-resistant and alkali-resistant and high scrub-resistant vinyl acetate-butyl acrylate emulsion as well as preparation of related coating |
| CN105482021A (en) * | 2016-01-19 | 2016-04-13 | 广东衡光化工有限公司 | Vac-veova emulsion with excellent comprehensive performance and preparation method of related coating |
| CN109824813A (en) * | 2018-12-12 | 2019-05-31 | 常熟巴德富科技有限公司 | A kind of acrylate and vinyl acetate emulsion and preparation method thereof |
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Application publication date: 20130612 |