CN108752601A - A kind of preparation method of phase inversion waterborne polyester lotion - Google Patents
A kind of preparation method of phase inversion waterborne polyester lotion Download PDFInfo
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- CN108752601A CN108752601A CN201810522401.1A CN201810522401A CN108752601A CN 108752601 A CN108752601 A CN 108752601A CN 201810522401 A CN201810522401 A CN 201810522401A CN 108752601 A CN108752601 A CN 108752601A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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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
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Cosmetics (AREA)
Abstract
The present invention provides a kind of preparation methods of phase inversion waterborne polyester lotion, include the following steps：1) 70-85 parts of branching type saturated polyester resins are warming up to 100-140 DEG C of suction filtration；2) filtered resin liquid is detected into solid content, when solid content is more than 95%, 1-1.5 parts of nonionic emulsifiers are added in the resin that step 1) obtains under stirring conditions, it controls solid content and is not less than 95%, 0.5-1.0 parts of anion emulsifiers are added after stirring, 1.5-2.5 parts of cosolvents are added after stirring；3) 30-50 parts of deionized waters are added at a slow speed in the mixture stirring obtained step 2), the speed of addition is 1-9L/min, when resin liquid is completely reformed into the opaque milk of milky by flowable transparent thick liquid, and viscosity is begun to decline, accelerate deionized water and speed is added, it controls as 2-18L/min to adding, continues to stir.A kind of preparation method of phase inversion waterborne polyester lotion provided by the invention is prepared that grain size is small, and stability is good by the control to emulsifying process, cost-effective lotion.
Description
Technical field
The present invention relates to a kind of waterborne polyester lotions, and in particular to a kind of preparation side of phase inversion waterborne polyester lotion
Method.
Background technology
In recent years, with national environmental consciousness be increasingly enhanced and national environmental protection policy it is increasingly strict, high VOC contains
Amount oil paint use be gradually restricted, and water paint rely on its low VOC content, the factors such as environmentally friendly, safe and healthy,
It is also increasingly wider using field, one of the main trend of the following paint field will be become.The performance of water-base resin/lotion is to water
Property coating influence it is great, currently, on the market water-base resin/product emulsion also in continuous upgrading optimization stage, quality and
Spread in performance is uneven, very big on the quality of downstream coating products, performance, feature of environmental protection influence, the exceeded "false" water of many voc occurs
Property coating products.In addition, since water paint price is higher compared with oil paint, and certain performances can't reach oil paint
Level, so the higher water-base resin/product emulsion of a collection of cost performance there is also certain limitation, is badly in need of in marketing.
In China industrial coating field, water paint proportion is also smaller at present, this is mainly by technology, price and political affairs
Plan regulation three aspect factor restricts.First, industrial coating field is (especially water-fast to the appearance, mechanical performance, patience of film
Property) etc. the requirements of performances be much higher than building inside and outside wall coating, and different application scenarios, it is desirable that different, China is former
Some first water paint technical merits can't generally meet requirement of the industrial coating to performance.Secondly, some performances are high
Water paint kind, due to being restricted by factors such as technique, scale and cost of material and sources, price is relatively high, this is also limited
Its extensive use is made.Furthermore in paint industry, if without special compulsive measures requirement, it is most by using inertia to be influenced
People is also reluctant that actively abandoning original has stablized the solvent based coating used and undertaken certain risk and go to use water paint, this also gives water
The popularization and application of property coating new product bring certain difficulty.
But in recent years, with the rapid economic development in our country, degree of opening further increases, with connecing for world economy
Are becoming tight rail and resource day and people are to environmentally friendly and health attention, water paint has welcome good hair in China
Opportunity is opened up, is generally acknowledged at present feature of environmental protection green coating kind.The development of water-base resin/lotion is relied in the development of water paint for counsel,
The progress of water-base resin/lotion necessarily promotes water paint progress.So needing a kind of oleoresin that can substitute high pollution
The higher water-soluble polyester resin with solvent content.
Invention content
The technical problem to be solved of the present invention is through the control to emulsifying process, and it is small to be prepared grain size, surely
A kind of qualitative good, cost-effective phase inversion waterborne polyester lotion.
The present invention solves above-mentioned technical problem using following technical scheme：
A kind of preparation method of phase inversion waterborne polyester lotion, includes the following steps：
1) 70-85 parts of branching type saturated polyester resins are warming up to 100-140 DEG C of suction filtration；
2) filtered resin liquid detection solid content is existed the resin that step 1) obtains when solid content is more than 95%
1-1.5 parts of nonionic emulsifiers are added under conditions of stirring, control solid content is not less than 95%, 0.5-1.0 parts are added after stirring
Anion emulsifier adds 1.5-2.5 parts of cosolvents after stirring；
3) 30-50 parts of deionized waters are added at a slow speed in the mixture stirring obtained step 2), and the speed of addition is 1-9L/
Min, when resin liquid is completely reformed into the opaque milk of milky by flowable transparent thick liquid, and viscosity is begun to decline, and is added
Speed is added in fast deionized water, controls as 2-18L/min to adding, continues to stir；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
Further, heating rate is 30-40 DEG C/h in the step 1).
Further, negative pressure is filtered in the step 1) be not less than 0.08Mpa.
Further, step 1) the branching type saturated polyester resin be branching type saturated polyester resin 3970E and
One or both of 8810x70.
Further, the step of detection solid content includes：The resin sampling 1.5-2g that step 1) obtains is taken, number is sampled
It is 2-4,1h is toasted in 150 DEG C of baking ovens after metering, then takes out weighing and calculate
Further, nonionic emulsifier is alkylphenol-polyethenoxy phenols nonionic emulsifier in the step 2).
Further, anion emulsifier is that alkyl diphenyl ether disulphonic acid sodium salt is anionic emulsifying in the step 2)
Agent.
Further, cosolvent is propylene glycol monomethyl ether in the step 2).
Further, nonionic emulsifier is NP-10 in the step 2), and anion emulsifier is in the step 2)
One or both of DOW-8390 and 2A1.
Further, stir speed (S.S.) is 30-80r/min in the step 2), mixture stirring speed in the step 3)
Rate is 30-80r/min, and the rate for continuing stirring is 200-400r/min.
The advantage of the invention is that：
1) a kind of preparation method of phase inversion waterborne polyester lotion provided by the invention obtains, using water as diluent,
Most volatile organic solvents in resin are substituted, VOC emission is greatly reduced, protects environment, protects contact personnel
Health, it is non-ignitable not quick-fried, avoid fire, risk of explosion；Simultaneously because water that is low using price, easily obtaining makees diluent, substitute
Dimethylbenzene equal solvent in oil paint, is greatly saved the energy, and meeting " energy-saving and emission-reduction " that current country implements, " clear water is green
Mountain " policy.
2) polyester resin that the present invention selects, by suction filtration, emulsifying process, by oiliness polyester resin in suitable compounding breast
Under agent, by the control to emulsifying process, reach that grain size is small, and stability is good, cost-effective lotion.
Specific implementation mode
It is described in detail below in conjunction with to the present invention.
Embodiment 1
A kind of preparation method of phase inversion waterborne polyester lotion, includes the following steps：
1) 80 parts of branching type saturated polyester resin 3970E are pumped into according to quantity in distillation still, are at the uniform velocity warming up to 120 DEG C of suction filtrations,
Heating rate is 30 DEG C/h；It filters negative pressure and is not less than 0.08Mpa；The organic solvent contained filters, condensing recovery extremely receives
Tank；
2) by filtered resin liquid sample detection solid content, test volume 1.5g, test sample number is 3, after metering
1h is toasted in 150 DEG C of baking ovens, weighing is then taken out and calculates, when solid content is more than 95%, filtered resin is put into special
In a mixing bowl, 1.2 parts of nonionic emulsifier NP-10 are added under stirring conditions, if solid content is less than 95%, continue to heat up
It filters, until qualified；0.6 part of anion emulsifier DOW-8390 is added in stirring after ten minutes, and stirring is added 2 parts after five minutes and helps
Solvent propylene glycol methyl ether；
3) mixture that step 2) obtains is continued into stirring and 32.2 parts of deionized waters is added after five minutes, the speed of addition is
1L/min observes resin phase transition state, when by original flowable transparent thick liquid to be completely reformed into milky impermeable for resin
Bright milk, and viscosity is begun to decline, and accelerates deionized water and speed is added, control as 2L/min to adding, when resin turns completely
It is melted into lotion, continues stirring 10 minutes；
Stir speed (S.S.) is 80r/min in step 2), and mixture stir speed (S.S.) is 80r/min in step 3), continues to stir
Rate be 400r/min；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
Embodiment 2
A kind of preparation method of phase inversion waterborne polyester lotion, includes the following steps：
1) 85 parts of branching type saturated polyester resin 3970E are pumped into according to quantity in distillation still, are at the uniform velocity warming up to 120 DEG C of suction filtrations,
Heating rate is 40 DEG C/h；It filters negative pressure and is not less than 0.08Mpa；The organic solvent contained filters, condensing recovery extremely receives
Tank；
2) by filtered resin liquid sample detection solid content, test volume 2g, test sample number is 3, after metering
150 DEG C of baking ovens toast 1h, then take out weighing and calculate, when solid content is more than 95%, filtered resin is put into special stir
It mixes in cylinder, 1.5 parts of nonionic emulsifier NP-10 is added under stirring conditions, if solid content is less than 95%, continues heating and take out
Filter, until qualified；0.75 part of anion emulsifier 2A1 is added in stirring after ten minutes, and 1.5 parts of cosolvents are added in stirring after five minutes
Propylene glycol monomethyl ether；
3) mixture that step 2) obtains is continued into stirring and 32.5 parts of deionized waters is added after five minutes, the speed of addition is
9L/min observes resin phase transition state, when by original flowable transparent thick liquid to be completely reformed into milky impermeable for resin
Bright milk, and viscosity is begun to decline, and accelerates deionized water and speed is added, control as 18L/min to adding, when resin turns completely
It is melted into lotion, continues stirring 10 minutes；
Stir speed (S.S.) is 30r/min in step 2), and mixture stir speed (S.S.) is 30r/min in step 3), continues to stir
Rate be 200r/min；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
Embodiment 3
A kind of preparation method of phase inversion waterborne polyester lotion, includes the following steps：
1) 70 parts of branching type saturated polyester resin 3970E are pumped into according to quantity in distillation still, are at the uniform velocity warming up to 100 DEG C of suction filtrations,
Heating rate is 30 DEG C/h；It filters negative pressure and is not less than 0.08Mpa；The organic solvent contained filters, condensing recovery extremely receives
Tank；
2) by filtered resin liquid sample detection solid content, test volume 1.5g, test sample number is 3, after metering
1h is toasted in 150 DEG C of baking ovens, weighing is then taken out and calculates, when solid content is more than 95%, filtered resin is put into special
In a mixing bowl, 1 part of nonionic emulsifier NP-10 is added under stirring conditions, if solid content is less than 95%, continues heating and takes out
Filter, until qualified；0.5 part of anion emulsifier DOW-8390 is added in stirring after 8 minutes, 1.5 parts of hydrotropies are added after 3 minutes in stirring
Agent propylene glycol monomethyl ether；
3) mixture that step 2) obtains is continued into stirring and 30 parts of deionized waters is added after five minutes, the speed of addition is 5L/
Min observes resin phase transition state, when resin is completely reformed into the opaque breast of milky by original flowable transparent thick liquid
Shape object, and viscosity is begun to decline, and accelerates deionized water and speed is added, control as 10L/min to adding, when resin is fully converted into
Lotion continues stirring 8 minutes；
Stir speed (S.S.) is 50r/min in step 2), and mixture stir speed (S.S.) is 60r/min in step 3), continues to stir
Rate be 200r/min；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
Embodiment 4
A kind of preparation method of phase inversion waterborne polyester lotion, includes the following steps：
1) 80 parts of branching type saturated polyester resin 8810x70 are pumped into according to quantity in distillation still, are at the uniform velocity warming up to 140 DEG C of pumpings
Filter, heating rate are 40 DEG C/h；It filters negative pressure and is not less than 0.08Mpa；The organic solvent that is contained filters, condensing recovery is to connecing
Closed cans；
2) by filtered resin liquid sample detection solid content, test volume 1.5g, test sample number is 3, after metering
1h is toasted in 150 DEG C of baking ovens, weighing is then taken out and calculates, when solid content is more than 95%, filtered resin is put into special
In a mixing bowl, 1.5 parts of nonionic emulsifier NP-10 are added under stirring conditions, if solid content is less than 95%, continue to heat up
It filters, until qualified；1.0 parts of anion emulsifier DOW-8390 are added in stirring after 12 minutes, stirring is added 2.5 parts after 7 minutes
Co-solvents propylene glycol methyl ether；
3) 50 parts of deionized waters are added after the mixture that step 2) obtains being continued stirring 7 minutes, the speed of addition is 6L/
Min observes resin phase transition state, when resin is completely reformed into the opaque breast of milky by original flowable transparent thick liquid
Shape object, and viscosity is begun to decline, and accelerates deionized water and speed is added, control as 12L/min to adding, when resin is fully converted into
Lotion continues stirring 12 minutes；
Stir speed (S.S.) is 50r/min in step 2), and mixture stir speed (S.S.) is 50r/min in step 3), continues to stir
Rate be 300r/min；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
Obtained phase inversion waterborne polyester emulsion technology index is as shown in the table in above-described embodiment：
Storage period：At 5-35 DEG C, 6 months.
Storage requirement：Storehouse drying, avoids being exposed to the sun, severe cold, freezes, drenches with rain shady and cool ventilation, forbids air storage.
This phase inversion waterborne polyester lotion is to convert preferred oiliness polyester resin to waterborne polyester lotion, is obtained
Waterborne polyester lotion VOC≤5%, meet national green environmental mark index request.And moisture content release property is good, initial stage water resistance
It is good.Gloss is high, and mechanical performance is excellent.The amino resins that can arrange in pairs or groups makes the drying baking vanish of 1K, can also mating aqueous isocyanic acid
Ester curing agent, makes 2K self-drying paints, and applicability is wide.
This phase inversion waterborne polyester lotion is mainly used for bicycle, electric vehicle, household electrical appliance and other instrument instrument
In the aqueous industrial baking vanish in the fields such as device；In the water-borne decorative anti-decaying paint that can also be used for various steel structure surfaces.
The foregoing is merely the preferred embodiments of the invention, are not intended to limit the invention creation, all at this
All any modification, equivalent and improvement etc., should be included in the invention made by within the spirit and principle of innovation and creation
Protection domain within.
Claims (10)
1. a kind of preparation method of phase inversion waterborne polyester lotion, which is characterized in that include the following steps：
1) 70-85 parts of branching type saturated polyester resins are warming up to 100-140 DEG C of suction filtration；
2) filtered resin liquid detection solid content is being stirred the resin that step 1) obtains when solid content is more than 95%
Under conditions of be added 1-1.5 part nonionic emulsifiers, control solid content be not less than 95%, after stirring be added 0.5-1.0 parts the moon from
Sub- emulsifier adds 1.5-2.5 parts of cosolvents after stirring；
3) 30-50 parts of deionized waters are added at a slow speed in the mixture stirring obtained step 2), and the speed of addition is 1-9L/min, when
Resin liquid is completely reformed into the opaque milk of milky by flowable transparent thick liquid, and viscosity is begun to decline, quickening go from
Speed is added in sub- water, controls as 2-18L/min to adding, continues to stir；
4) sample detection filters packaging of weighing after qualified；The each component raw material is in parts by weight.
2. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
It is rapid 1) in heating rate be 30-40 DEG C/h.
3. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
Rapid 1) the middle negative pressure that filters is not less than 0.08Mpa.
4. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
Rapid 1) branching type saturated polyester resin is one or both of branching type saturated polyester resin 3970E and 8810x70.
5. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the inspection
Survey solid content the step of include：The resin sampling 1.5-2g that step 1) obtains is taken, sampling number is 2-4, is dried at 150 DEG C after metering
Case toasts 1h, then takes out weighing and calculates.
6. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
It is rapid 2) in nonionic emulsifier be alkylphenol-polyethenoxy phenols nonionic emulsifier.
7. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
It is rapid 2) in anion emulsifier be alkyl diphenyl ether disulphonic acid sodium salt anion emulsifier.
8. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
It is rapid 2) in cosolvent be propylene glycol monomethyl ether.
9. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that the step
It is rapid 2) in nonionic emulsifier be NP-10, anion emulsifier is one kind or two in DOW-8390 and 2A1 in the step 2)
Kind.
10. a kind of preparation method of phase inversion waterborne polyester lotion according to claim 1, which is characterized in that described
Stir speed (S.S.) is 30-80r/min in step 2), and mixture stir speed (S.S.) is 30-80r/min in the step 3), continues to stir
The rate mixed is 200-400r/min.
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| CN201810522401.1A CN108752601A (en) | 2018-05-28 | 2018-05-28 | A kind of preparation method of phase inversion waterborne polyester lotion |
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| CN201810522401.1A CN108752601A (en) | 2018-05-28 | 2018-05-28 | A kind of preparation method of phase inversion waterborne polyester lotion |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104530399A (en) * | 2014-12-18 | 2015-04-22 | 青岛乐化科技有限公司 | Preparation method of zero-VOC high-performance alcoholic acid emulsion |
| CN105623203A (en) * | 2014-11-26 | 2016-06-01 | 邢国爱 | Resin emulsion |
| CN107446472A (en) * | 2017-08-04 | 2017-12-08 | 合众（佛山）化工有限公司 | A kind of waterborne polyester coating modified unsaturated polyester emulsion and preparation method thereof |
-
2018
- 2018-05-28 CN CN201810522401.1A patent/CN108752601A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105623203A (en) * | 2014-11-26 | 2016-06-01 | 邢国爱 | Resin emulsion |
| CN104530399A (en) * | 2014-12-18 | 2015-04-22 | 青岛乐化科技有限公司 | Preparation method of zero-VOC high-performance alcoholic acid emulsion |
| CN107446472A (en) * | 2017-08-04 | 2017-12-08 | 合众（佛山）化工有限公司 | A kind of waterborne polyester coating modified unsaturated polyester emulsion and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 郑常杏 等: ""相反转法制备水性醇酸树脂"", 《上海涂料》 * |
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Application publication date: 20181106 |