CN108250455A - A kind of aqueous saturated polyester resin dispersion emulsion and preparation method thereof - Google Patents
A kind of aqueous saturated polyester resin dispersion emulsion and preparation method thereof Download PDFInfo
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- CN108250455A CN108250455A CN201810029463.9A CN201810029463A CN108250455A CN 108250455 A CN108250455 A CN 108250455A CN 201810029463 A CN201810029463 A CN 201810029463A CN 108250455 A CN108250455 A CN 108250455A
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- polyester resin
- saturated polyester
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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
- 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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- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of aqueous saturated polyester resin dispersion emulsions and preparation method thereof.It is described, it is made of the raw material of following parts by weight：Saturated polyester resin：50 60 parts, nonionic emulsifier：0.5 2.5 parts, anion emulsifier：0.5 2.5 parts, deionized water：40 50 parts.The invention has the advantages that：VOC content is extremely low, dispersion effect is good, storage time is long.
Description
Technical field
The present invention relates to a kind of dispersion emulsion and preparation method thereof, specifically a kind of aqueous saturated polyester resin dispersion breast
Liquid and preparation method thereof.
Background technology
Significant industry of the automobile industry as modernized society, with the high speed development of China's economic, has become state
The pillar industry of people's economy.However, its negative effect generated to environment also further highlights, the vehicle of present domestic automobile industry
Spray painting generally use low-solid-content solvent based coating, the production of solvent based coating and work progress all can be arranged inevitably
The organic compound of amplification quantity（VOC）And hazardous air pollutants（), HAPS this will seriously endanger human health and causes environment
Pollution.Therefore, the standard GB24409-2009 promulgated in country in 2010《Limits of harmful substances in car paint》Also stringent limit
The discharge capacity of car paint VOC is made.For meet the requirement of environmental protection and push sustainable, the environmentally protective development of automobile industry,
Car paint just develops towards high solid, powdery paints and Water-borne modification direction, and wherein Water-borne modification is most effective
Approach.Solvent type saturated polyester amino-stoving varnish is the major product of car paint, accounts for about 60 parts of entire car paint dosage --
70 parts, VOC content reaches 125g/L, and the VOC content of aqueous saturated polyester amino-stoving varnish only has 25g/L, but aqueous saturation is gathered
Ester amino-stoving varnish relies on import always now.Therefore, one that aqueous saturated polyester amino-stoving varnish is domestic coating industry is developed
The scientific research mission of the task of top priority.In aqueous saturated polyester amino-stoving varnish, it is wherein crucial skill to research and develop aqueous saturated polyester resin
Art.
The resting period of current aqueous saturated polyester resin dispersion emulsion generally between 6 months to 12 months, during storage
Between do not grow generally, which results in aqueous saturated polyester resin dispersion emulsions to need to use as early as possible after production, newborn as time go on
The effect of liquid gradually reduces, and the needs of the material strictly need to be controlled which results in production and using producer, increase enterprise
Management and control cost, while also high to the transport of material requirement, and be used as its transport requirement of industrial chemicals, cause the raw material production or
Use cost increases.
Invention content
The technical problems to be solved by the invention are to provide the aqueous saturated polyester that a kind of VOC content is low, and storage time is grown
Resin dispersion lotion and preparation method thereof.
In order to solve the above technical problems, the technical scheme is that：A kind of aqueous saturated polyester resin dispersion emulsion, by
The raw material of following parts by weight is made：Saturated polyester resin：50-60 parts, nonionic emulsifier：It is 0.5-2.5 parts, anionic emulsifying
Agent：0.5-2.5 parts, deionized water：40-50 parts.
As preferred technical solution, a kind of aqueous saturated polyester resin dispersion emulsion, by following raw material
It is made：Saturated polyester resin：55 parts, nonionic emulsifier：1.5 parts, anion emulsifier：1.5 parts, deionized water：45 parts.
The present invention also provides a kind of above-mentioned production method of aqueous saturated polyester resin dispersion emulsion, including following step
Suddenly：
Step 1：Water purification is heated to 80-90 DEG C by the preparation of deionized water, maintains the temperature then in turn through multimedium mistake
Filter → active carbon filter → accurate filter, by the water after filtering near 4-6 DEG C in 5-8 minutes, then by reverse osmosis
It is spare to be filled to ultraviolet light water tank by saturating equipment processing after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 60 DEG C -70 DEG C, is put into the dispersion bottle for being equipped with blender, disperses bottle
It is put into 60 DEG C -70 DEG C of thermostatical water bath, opens stirring, rotating speed is controlled in 100r/min, by nonionic emulsifier, anion breast
Agent is put into dispersion bottle, keeps the temperature 30min；
Step 3：Then 60 DEG C of -70 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.
When deionized water adds in 50%-60%, saturated polyester resin dispersion liquid starts to bleach, and is water packet by original Water-In-Oil phase inversion
Oil continuously adds remaining deionized water, then keeps the temperature 1 hour at 60 DEG C -70 DEG C, obtains aqueous saturated polyester resin dispersion
Liquid.
Preferably, the resistance value of the deionized water is 100,000 ohm.
Preferably, the nonionic emulsifier, anion emulsifier are produced for CROD companies of Britain.
Preferably, 92 parts of the solid holdup of the saturated polyester resin.
By adopting the above-described technical solution, a kind of aqueous saturated polyester resin dispersion emulsion, by following raw material
It is made：Saturated polyester resin：50-60 parts, nonionic emulsifier：0.5-2.5 parts, anion emulsifier：0.5-2.5 parts, go from
Sub- water：40-50 parts；The invention has the advantages that：
1st, the VOC content of aqueous saturated polyester resin dispersion emulsion is extremely low.What the aqueous saturated polyester resin dispersion emulsion was prepared
Aqueous saturated polyester amino vehicle baking vanish using water as diluent, effectively reduces the content of VOC in car paint, makes
Aqueous saturated polyester amino vehicle baking vanish pollution-free nonhazardous in spraying process is obtained, greatly improves construction environment and automobile
The discharge capacity of the entire VOC of factory belongs to green product, and the VOC included in every liter of aqueous saturated polyester resin dispersion emulsion is not
More than 50g/L.
2nd, dispersion effect is good, the range smaller of the dispersion particle diameter of aqueous saturated polyester resin dispersion emulsion, particle diameter distribution model
It encloses and narrows, dispersion particle diameter 200--1000nm.
3rd, the resting period is long, and the solid content of aqueous saturated polyester dispersion emulsion improves, and reduces aqueous saturated polyester tree
The solvent content of fat dispersion emulsion, while the aqueous saturated polyester resin dispersion emulsion is increased, in 55 DEG C of heat preservation oven
The stability of the change of size of the storage of storage 260 days stores the change of size of the storage of 480 days in 40 DEG C of heat preservation oven
Stability.
Specific embodiment
The present invention is described further with reference to specific embodiment.
Embodiment 1
A kind of aqueous saturated polyester resin dispersion emulsion, is made of following raw material：Saturated polyester resin：50 parts, it is non-from
Sub- emulsifier：0.5 part, anion emulsifier：0.5 part, deionized water：40 parts.
The resistance value of the deionized water is 100,000 ohm, and the nonionic emulsifier, anion emulsifier are Britain
CROD companies produce, 92 parts of the solid holdup of the saturated polyester resin.
A kind of production method of above-mentioned aqueous saturated polyester resin dispersion emulsion, includes the following steps：
Step 1：Water purification is heated to 80 DEG C by the preparation of deionized water, maintains the temperature then in turn through more medium filter
→ active carbon filter → accurate filter, by near 4 DEG C in 5 minutes of the water after filtering, then by reverse osmosis equipment at
It is spare to be filled to ultraviolet light water tank by reason after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 60 DEG C, is put into the dispersion bottle for being equipped with blender, dispersion bottle is put into 60
DEG C thermostatical water bath in, open stirring, rotating speed control is put into nonionic emulsifier, anion emulsifier in 100r/min
Disperse in bottle, keep the temperature 30min；
Step 3：Then 60 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.When go from
When sub- water adds in 50%, saturated polyester resin dispersion liquid starts to bleach, and is oil-in-water by original Water-In-Oil phase inversion, continuously adds
Then remaining deionized water keeps the temperature 1 hour at 60 DEG C, obtains aqueous saturated polyester resin dispersion liquid.
The aqueous saturated polyester resin dispersion liquid that this example 1 is made, is detected grain size and particle diameter distribution, test result
It is as follows：
1. grain size：200--1000nm；
2. particle diameter distribution：It is bimodal；
3. it is stored 260 days in 55 DEG C of heat preservation oven, grain size 200nm--1000nm；
It is stored 480 days in 4.40 DEG C of heat preservation oven, grain size 200nm--1000nm；
5.VOC contents are 40g/L.
Embodiment 2
A kind of aqueous saturated polyester resin dispersion emulsion, is made of following raw material：Saturated polyester resin：60 parts, it is non-from
Sub- emulsifier：2.5 parts, anion emulsifier：2.5 parts, deionized water：50 parts.
The resistance value of the deionized water is 100,000 ohm, and the nonionic emulsifier, anion emulsifier are Britain
CROD companies produce, 92 parts of the solid holdup of the saturated polyester resin.
A kind of production method of above-mentioned aqueous saturated polyester resin dispersion emulsion, includes the following steps：
Step 1：Water purification is heated to 90 DEG C by the preparation of deionized water, maintains the temperature then in turn through more medium filter
→ active carbon filter → accurate filter, by the water after filtering near 6 DEG C in 8 minutes, then by reverse osmosis equipment at
It is spare to be filled to ultraviolet light water tank by reason after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 70 DEG C, is put into the dispersion bottle for being equipped with blender, dispersion bottle is put into 70
DEG C thermostatical water bath in, open stirring, rotating speed control is put into nonionic emulsifier, anion emulsifier in 100r/min
Disperse in bottle, keep the temperature 30min；
Step 3：Then 70 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.When go from
When sub- water adds in 60%, saturated polyester resin dispersion liquid starts to bleach, and is oil-in-water by original Water-In-Oil phase inversion, continuously adds
Then remaining deionized water keeps the temperature 1 hour at 70 DEG C, obtains aqueous saturated polyester resin dispersion liquid.
The aqueous saturated polyester resin dispersion liquid that this example 2 is made, is detected grain size and particle diameter distribution, test result
It is as follows：
1. grain size：200--500nm
2. particle diameter distribution：It is unimodal
3. it is stored 250 days in 55 DEG C of heat preservation oven, grain size 200nm--500nm；
4. it is stored 440 days in 40 DEG C of heat preservation oven, grain size 200nm--500nm；
5.VOC contents are 48g/L.
Embodiment 3
A kind of aqueous saturated polyester resin dispersion emulsion, is made of following raw material：Saturated polyester resin：55 parts, it is non-from
Sub- emulsifier：1.5 parts, anion emulsifier：1.5 parts, deionized water：45 parts.
The resistance value of the deionized water is 100,000 ohm, and the nonionic emulsifier, anion emulsifier are Britain
CROD companies produce, 92 parts of the solid holdup of the saturated polyester resin.
A kind of production method of above-mentioned aqueous saturated polyester resin dispersion emulsion, includes the following steps：
Step 1：Water purification is heated to 85 DEG C by the preparation of deionized water, maintains the temperature then in turn through more medium filter
→ active carbon filter → accurate filter, by the water after filtering near 5 DEG C in 6.5 minutes, then by reverse osmosis equipment
It is spare to be filled to ultraviolet light water tank by processing after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 65 DEG C, is put into the dispersion bottle for being equipped with blender, dispersion bottle is put into 65
DEG C thermostatical water bath in, open stirring, rotating speed control is put into nonionic emulsifier, anion emulsifier in 100r/min
Disperse in bottle, keep the temperature 30min；
Step 3：Then 65 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.When go from
When sub- water adds in 55%, saturated polyester resin dispersion liquid starts to bleach, and is oil-in-water by original Water-In-Oil phase inversion, continuously adds
Then remaining deionized water keeps the temperature 1 hour at 65 DEG C, obtains aqueous saturated polyester resin dispersion liquid.
The aqueous saturated polyester resin dispersion liquid that this example 3 is made, is detected grain size and particle diameter distribution, test result
It is as follows：
1. grain size：200--500nm；
2. particle diameter distribution：It is unimodal；
3. it is stored 266 days in 55 DEG C of heat preservation oven, grain size 200nm--500nm；
4. it is stored 500 days in 40 DEG C of heat preservation oven, grain size 200nm--500nm；
5.VOC contents are 44g/L.
Embodiment 4
A kind of aqueous saturated polyester resin dispersion emulsion, is made of following raw material：Saturated polyester resin：Saturated polyester tree
Fat：52 parts, nonionic emulsifier：1 part, anion emulsifier：1 part, deionized water：43 parts.
The resistance value of the deionized water is 100,000 ohm, and the nonionic emulsifier, anion emulsifier are Britain
CROD companies produce, 92 parts of the solid holdup of the saturated polyester resin.
A kind of production method of above-mentioned aqueous saturated polyester resin dispersion emulsion, includes the following steps：
Step 1：Water purification is heated to 83 DEG C by the preparation of deionized water, maintains the temperature then in turn through more medium filter
→ active carbon filter → accurate filter, by the water after filtering near 4 DEG C in 7 minutes, then by reverse osmosis equipment at
It is spare to be filled to ultraviolet light water tank by reason after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 68 DEG C, is put into the dispersion bottle for being equipped with blender, dispersion bottle is put into 68
DEG C thermostatical water bath in, open stirring, rotating speed control is put into nonionic emulsifier, anion emulsifier in 100r/min
Disperse in bottle, keep the temperature 30min；
Step 3：Then 68 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.When go from
When sub- water adds in 57%, saturated polyester resin dispersion liquid starts to bleach, and is oil-in-water by original Water-In-Oil phase inversion, continuously adds
Then remaining deionized water keeps the temperature 1 hour at 66 DEG C, obtains aqueous saturated polyester resin dispersion liquid.
The aqueous saturated polyester resin dispersion liquid that this example 4 is made, is detected grain size and particle diameter distribution, test result
It is as follows：
1. grain size：200--500nm；
2. particle diameter distribution：It is unimodal；
3. it is stored 270 days in 55 DEG C of heat preservation oven, grain size 200nm--500nm；
4. it is stored 540 days in 40 DEG C of heat preservation oven, grain size 200nm--500nm；
5.VOC contents are 41.6g/L.
The foregoing is merely the schematical specific embodiments of the present invention, are not limited to the scope of the present invention.It is any
Those skilled in the art, made equivalent variations and modification under the premise of the design of the present invention and principle is not departed from,
The scope of protection of the invention should be belonged to.
Claims (6)
1. a kind of aqueous saturated polyester resin dispersion emulsion, which is characterized in that be made of the raw material of following parts by weight：Saturated polyester
Resin：50-60 parts, nonionic emulsifier：0.5-2.5 parts, anion emulsifier：0.5-2.5 parts, deionized water：40-50 parts.
2. a kind of aqueous saturated polyester resin dispersion emulsion as described in claim 1, which is characterized in that by following parts by weight
Raw material is made：Saturated polyester resin：55 parts, nonionic emulsifier：1.5 parts, anion emulsifier：1.5 parts, deionized water：45
Part.
3. a kind of production method of aqueous saturated polyester resin dispersion emulsion as claimed in claim 1 or 2, which is characterized in that
Include the following steps：
Step 1：Water purification is heated to 80-90 DEG C by the preparation of deionized water, maintains the temperature then in turn through multimedium mistake
Filter → active carbon filter → accurate filter, by the water after filtering near 4-6 DEG C in 5-8 minutes, then by reverse osmosis
It is spare to be filled to ultraviolet light water tank by saturating equipment processing after the completion of processing for the deionized water of acquisition；
Step 2：Saturated polyester resin is heated to 60 DEG C -70 DEG C, is put into the dispersion bottle for being equipped with blender, disperses bottle
It is put into 60 DEG C -70 DEG C of thermostatical water bath, opens stirring, rotating speed is controlled in 100r/min, by nonionic emulsifier, anion breast
Agent is put into dispersion bottle, keeps the temperature 30min；
Step 3：Then 60 DEG C of -70 DEG C of deionized waters are would be heated to, are added in saturated polyester resin with the speed of 1g/min.
When deionized water adds in 50%-60%, saturated polyester resin dispersion liquid starts to bleach, and is water packet by original Water-In-Oil phase inversion
Oil continuously adds remaining deionized water, then keeps the temperature 1 hour at 60 DEG C -70 DEG C, obtains aqueous saturated polyester resin dispersion
Liquid.
4. a kind of aqueous saturated polyester resin dispersion emulsion as claimed in claim 1 or 2, it is characterised in that：The deionization
The resistance value of water is 100,000 ohm.
5. a kind of aqueous saturated polyester resin dispersion emulsion as claimed in claim 1 or 2, it is characterised in that：The nonionic
Emulsifier, anion emulsifier are produced for CROD companies of Britain.
6. a kind of aqueous saturated polyester resin dispersion emulsion as claimed in claim 1 or 2, it is characterised in that：The saturation is gathered
92 parts of the solid holdup of ester resin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810029463.9A CN108250455A (en) | 2018-01-12 | 2018-01-12 | A kind of aqueous saturated polyester resin dispersion emulsion and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810029463.9A CN108250455A (en) | 2018-01-12 | 2018-01-12 | A kind of aqueous saturated polyester resin dispersion emulsion and preparation method thereof |
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| CN108250455A true CN108250455A (en) | 2018-07-06 |
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ID=62726968
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006249391A (en) * | 2005-03-14 | 2006-09-21 | Toyota Motor Corp | Water-based dispersion-slurry coating |
| CN104045761A (en) * | 2014-06-16 | 2014-09-17 | 张家港康得新光电材料有限公司 | Matte scratch-resistant water-based resin and preparation method thereof |
| WO2015154157A1 (en) * | 2014-04-08 | 2015-10-15 | Oxiteno S.A. Indústria E Comércio | Resin emulsion composition and method for producing same |
-
2018
- 2018-01-12 CN CN201810029463.9A patent/CN108250455A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006249391A (en) * | 2005-03-14 | 2006-09-21 | Toyota Motor Corp | Water-based dispersion-slurry coating |
| WO2015154157A1 (en) * | 2014-04-08 | 2015-10-15 | Oxiteno S.A. Indústria E Comércio | Resin emulsion composition and method for producing same |
| CN104045761A (en) * | 2014-06-16 | 2014-09-17 | 张家港康得新光电材料有限公司 | Matte scratch-resistant water-based resin and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| 万小婷 等: "核壳结构叔丙乳液的合成及其稳定性影响的研究", 《涂料工业》 * |
| 习娟 等: "转相乳化法制备零VOC水性醇酸乳液的实验研究", 《宁夏师范学院学报（自然科学）》 * |
| 刘微微 等: "《现代电泳涂装百科全书》", 31 December 2016, 复旦大学出版社 * |
| 曾作祥: "《界面现象》", 31 January 2016, 华东理工大学出版社 * |
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Application publication date: 20180706 |