CN105461845A - Method for synthesizing ultraviolet-resistance compound emulsion - Google Patents
Method for synthesizing ultraviolet-resistance compound emulsion Download PDFInfo
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- CN105461845A CN105461845A CN201510990550.7A CN201510990550A CN105461845A CN 105461845 A CN105461845 A CN 105461845A CN 201510990550 A CN201510990550 A CN 201510990550A CN 105461845 A CN105461845 A CN 105461845A
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- emulsion
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- boiling flask
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- uvioresistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F216/00—Copolymers 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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical
- C08F216/12—Copolymers 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 an alcohol, ether, aldehydo, ketonic, acetal or ketal radical by an ether radical
- C08F216/14—Monomers containing only one unsaturated aliphatic radical
- C08F216/1416—Monomers containing oxygen in addition to the ether oxygen, e.g. allyl glycidyl ether
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D129/00—Coating compositions based on homopolymers or copolymers 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/10—Homopolymers or copolymers of unsaturated ethers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers 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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/02—Homopolymers or copolymers of acids; Metal or ammonium salts thereof
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to a method for synthesizing an ultraviolet-resistance compound emulsion. The method comprises the following steps: polymerizing in a four-neck flask which is provided with a condenser pipe, a dropping device, an electronic stirring bar and an automatic temperature-control water-bath kettle; dissolving compound emulsifier in water, and dividing the solution into two parts, stirring one part in the four-neck flask for later use, and preparing an pre-emulsion from the other part and a mixed monomer of methyl methacrylate, butyl acrylate, acrylic acid and 2-hydroxy-4-propenyloxy benzophenone mixed monomer; simultaneously adding the initiator and the pre-emulsion into the four-neck flask, controlling temperature, and initiating polymerization to prepare seed emulsion; adding the rest pre-emulsion and initiator when the seed emulsion turns blue, keeping on reaction after dripping is finished, and stopping heating and stirring; and cooling to perform post-elimination treatment, cooling to room temperature, regulating the pH value of ammonia hydroxide, filtering, and discharging to obtain the ultraviolet-proofing silicone acrylic emulsion. The method is simple and is easy to control, and the synthesized silicone acrylic emulsion has excellent temperature change resistance, weather resistance and ultraviolet resistance.
Description
Technical field
The present invention relates to the synthetic technology of a kind of organic coating preparation materials, particularly relate to a kind of uvioresistant composite emulsion synthetic method.
Background technology
Acrylic emulsion has the advantages such as good temperature-change resistance, weathering resistance, water tolerance, hardness, is a kind of high performance outer wall paint emulsion, is widely used in fields such as building and decorations.But the acrylic emulsion of technique synthesis at present, anti-uv-ray is still more weak, the over-all properties of coating prepared by extreme influence acrylic emulsion, and the life cycle of brick coating imitated by serious curtailment exterior wall, therefore improve synthesis technique, improve acrylic emulsion anti-uv-ray and seem particularly important.
Summary of the invention
It is simple that technical problem to be solved by this invention is to provide a kind of method, easy to control, and the organosilicon crylic acid latex of synthesis has the synthetic method of excellent temperature-change resistance, weathering resistance, uvioresistant ability.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of uvioresistant composite emulsion synthetic method, comprises the steps:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath;
Compound emulsifying agent is water-soluble and be divided into two parts, and portion is placed in four-hole boiling flask and stirs stand-by, and another part and methyl methacrylate, butyl acrylate, vinylformic acid, 2 monohydroxy 1 propenyloxy group benzophenone mix monomers obtain pre-emulsion;
Initiator, pre-emulsion are added in four-hole boiling flask, control temperature, initiated polymerization prepares seed emulsion simultaneously;
When seed emulsion starts to become blue, adding remaining pre-emulsion and initiator, dripping off rear continuation reaction, stopping heating and stir;
Lower the temperature and carry out rear Processing for removing, being down to room temperature, using ammoniacal liquor adjust ph, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described that compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains being implemented as follows of pre-emulsion step with methyl methacrylate, butyl acrylate, vinylformic acid, 2 monohydroxy 1 propenyloxy group benzophenone mix monomers:
Compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains pre-emulsion with the methyl methacrylate of 1 ~ 3%, butyl acrylate, the vinylformic acid of 6 ~ 9%, the 2 monohydroxy 1 propenyloxy group benzophenone mix monomers of 6 ~ 10% of 3 ~ 6%.
Further, describedly initiator, pre-emulsion to be added in four-hole boiling flask, control temperature, initiated polymerization prepares being implemented as follows of seed emulsion step simultaneously:
30 ~ 50% initiators, 5 ~ 10% pre-emulsions are added in four-hole boiling flask, control temperature is 70 ~ 80 DEG C, and initiated polymerization prepares seed emulsion simultaneously.
Further, describedly start to become blue when seed emulsion, adding remaining pre-emulsion and initiator, dripping off rear continuations reaction, stop heating and being implemented as follows of whipping step:
Question response carries out 1 ~ 2h, and seed emulsion starts to become blue, then adds remaining 90 ~ 95% pre-emulsions and 50 ~ 70% initiators, and 3 ~ 4h drips off rear continuation reaction 0.1 ~ 1h, stops heating and stirs 10 ~ 30min.
Further, described cooling also carries out rear Processing for removing, is down to room temperature, uses ammoniacal liquor adjust ph, and filter, discharging, obtains being implemented as follows of uvioresistant organosilicon crylic acid latex step:
Lower the temperature and carry out rear Processing for removing, being down to room temperature, by ammoniacal liquor adjust ph 7 ~ 8, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
The invention has the beneficial effects as follows: method is simple, easy to control, the organosilicon crylic acid latex of synthesis has excellent temperature-change resistance, weathering resistance, uvioresistant ability.
Embodiment
Be described principle of the present invention and feature below in conjunction with example, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A kind of uvioresistant composite emulsion synthetic method, comprises the steps:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath;
Compound emulsifying agent is water-soluble and be divided into two parts, and portion is placed in four-hole boiling flask and stirs stand-by, and another part and methyl methacrylate, butyl acrylate, vinylformic acid, 2 monohydroxy 1 propenyloxy group benzophenone mix monomers obtain pre-emulsion;
Initiator, pre-emulsion are added in four-hole boiling flask, control temperature, initiated polymerization prepares seed emulsion simultaneously;
When seed emulsion starts to become blue, adding remaining pre-emulsion and initiator, dripping off rear continuation reaction, stopping heating and stir;
Lower the temperature and carry out rear Processing for removing, being down to room temperature, using ammoniacal liquor adjust ph, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
Embodiment 1:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath; Compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains pre-emulsion with the methyl methacrylate of 1%, butyl acrylate, the vinylformic acid of 6%, the 2 monohydroxy 1 propenyloxy group benzophenone mix monomers of 6% of 3%; 30% initiator, 5% pre-emulsion are added in four-hole boiling flask, control temperature is 70 DEG C, and initiated polymerization prepares seed emulsion simultaneously; Question response carries out 1h, and seed emulsion starts to become blue, then adds remaining 90% pre-emulsion and 50% initiator, and 3h drips off rear continuation reaction 0.1h, stops heating and stirs 10min; Lower the temperature and carry out rear Processing for removing, being down to room temperature, by ammoniacal liquor adjust ph 7, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
Embodiment 2:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath; Compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains pre-emulsion with the methyl methacrylate of 2%, butyl acrylate, the vinylformic acid of 8%, the 2 monohydroxy 1 propenyloxy group benzophenone mix monomers of 8% of 5%; 35% initiator, 6% pre-emulsion are added in four-hole boiling flask, control temperature is 75 DEG C, and initiated polymerization prepares seed emulsion simultaneously; Question response carries out 1.5h, and seed emulsion starts to become blue, then adds remaining 92% pre-emulsion and 60% initiator, and 3.5h drips off rear continuation reaction 0.6h, stops heating and stirs 20min; Lower the temperature and carry out rear Processing for removing, being down to room temperature, by ammoniacal liquor adjust ph 7.5, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
Embodiment 3:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath; Compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains pre-emulsion with the methyl methacrylate of 3%, butyl acrylate, the vinylformic acid of 9%, the 2 monohydroxy 1 propenyloxy group benzophenone mix monomers of 10% of 6%; 50% initiator, 10% pre-emulsion are added in four-hole boiling flask, control temperature is 80 DEG C, and initiated polymerization prepares seed emulsion simultaneously; Question response carries out 2h, and seed emulsion starts to become blue, then adds remaining 95% pre-emulsion and 70% initiator, and 4h drips off rear continuation reaction 1h, stops heating and stirs 30min; Lower the temperature and carry out rear Processing for removing, being down to room temperature, by ammoniacal liquor adjust ph 8, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a uvioresistant composite emulsion synthetic method, is characterized in that, comprises the steps:
In four-hole boiling flask, carry out polyreaction, whole device is with prolong, Dropping feeder, driven stirring rod and temperature automatically controlled water-bath;
Compound emulsifying agent is water-soluble and be divided into two parts, and portion is placed in four-hole boiling flask and stirs stand-by, and another part and methyl methacrylate, butyl acrylate, vinylformic acid, 2 monohydroxy 1 propenyloxy group benzophenone mix monomers obtain pre-emulsion;
Initiator, pre-emulsion are added in four-hole boiling flask, control temperature, initiated polymerization prepares seed emulsion simultaneously;
When seed emulsion starts to become blue, adding remaining pre-emulsion and initiator, dripping off rear continuation reaction, stopping heating and stir;
Lower the temperature and carry out rear Processing for removing, being down to room temperature, using ammoniacal liquor adjust ph, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
2. a kind of uvioresistant composite emulsion synthetic method according to claim 1, it is characterized in that, described that compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains being implemented as follows of pre-emulsion step with methyl methacrylate, butyl acrylate, vinylformic acid, 2 monohydroxy 1 propenyloxy group benzophenone mix monomers:
Compound emulsifying agent is water-soluble and be divided into two parts, portion is placed in four-hole boiling flask and stirs stand-by, and another part obtains pre-emulsion with the methyl methacrylate of 1 ~ 3%, butyl acrylate, the vinylformic acid of 6 ~ 9%, the 2 monohydroxy 1 propenyloxy group benzophenone mix monomers of 6 ~ 10% of 3 ~ 6%.
3. a kind of uvioresistant composite emulsion synthetic method according to claim 1, is characterized in that, describedly initiator, pre-emulsion is added in four-hole boiling flask simultaneously, control temperature, and initiated polymerization prepares being implemented as follows of seed emulsion step:
30 ~ 50% initiators, 5 ~ 10% pre-emulsions are added in four-hole boiling flask, control temperature is 70 ~ 80 DEG C, and initiated polymerization prepares seed emulsion simultaneously.
4. a kind of uvioresistant composite emulsion synthetic method according to claim 1, is characterized in that, describedly starts to become blue when seed emulsion, is adding remaining pre-emulsion and initiator, is dripping off rear continuations reaction, stops heating and being implemented as follows of whipping step:
Question response carries out 1 ~ 2h, and seed emulsion starts to become blue, then adds remaining 90 ~ 95% pre-emulsions and 50 ~ 70% initiators, and 3 ~ 4h drips off rear continuation reaction 0.1 ~ 1h, stops heating and stirs 10 ~ 30min.
5. a kind of uvioresistant composite emulsion synthetic method according to claim 1, it is characterized in that, described cooling also carries out rear Processing for removing, is down to room temperature, uses ammoniacal liquor adjust ph, and filter, discharging, obtains being implemented as follows of uvioresistant organosilicon crylic acid latex step:
Lower the temperature and carry out rear Processing for removing, being down to room temperature, by ammoniacal liquor adjust ph 7 ~ 8, filter, discharging, obtains uvioresistant organosilicon crylic acid latex.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510990550.7A CN105461845A (en) | 2015-12-25 | 2015-12-25 | Method for synthesizing ultraviolet-resistance compound emulsion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510990550.7A CN105461845A (en) | 2015-12-25 | 2015-12-25 | Method for synthesizing ultraviolet-resistance compound emulsion |
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| Publication Number | Publication Date |
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| CN105461845A true CN105461845A (en) | 2016-04-06 |
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| CN201510990550.7A Pending CN105461845A (en) | 2015-12-25 | 2015-12-25 | Method for synthesizing ultraviolet-resistance compound emulsion |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116194539A (en) * | 2020-07-02 | 2023-05-30 | 贝洱工艺公司 | Stain resistant latex resin |
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2015
- 2015-12-25 CN CN201510990550.7A patent/CN105461845A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116194539A (en) * | 2020-07-02 | 2023-05-30 | 贝洱工艺公司 | Stain resistant latex resin |
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Application publication date: 20160406 |