CN108948942A - A kind of two-component transparent fire-resisting paint of high impact properties and preparation method thereof - Google Patents
A kind of two-component transparent fire-resisting paint of high impact properties and preparation method thereof Download PDFInfo
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- CN108948942A CN108948942A CN201810831482.3A CN201810831482A CN108948942A CN 108948942 A CN108948942 A CN 108948942A CN 201810831482 A CN201810831482 A CN 201810831482A CN 108948942 A CN108948942 A CN 108948942A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
- C08G14/10—Melamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/12—Chemically modified polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1405—Polycondensates modified by chemical after-treatment with inorganic compounds
- C08G59/1422—Polycondensates modified by chemical after-treatment with inorganic compounds containing phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/14—Polycondensates modified by chemical after-treatment
- C08G59/1433—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
- C08G59/1477—Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/62—Alcohols or phenols
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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
- C09D161/00—Coating compositions based on condensation polymers of aldehydes or ketones; Coating compositions based on derivatives of such polymers
- C09D161/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C09D161/04, C09D161/18 and C09D161/20
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention relates to two-component transparent fire-resisting paints of a kind of high impact properties and preparation method thereof, belong to functional paint scope.Headed by specific step first using solid formaldehyde, melamine, pentaerythrite, urea as the amino resins of Material synthesis low content of free formaldehyde be component A as film forming matter, B component is phosphoric acid, epoxy resin, a kind of phosphate that urea, polyethylene glycol are prepared by solwution method, then it is stirred with water-compatible amino resin different proportion, the aqueous transparent fireproof coating of two-component can be obtained.Coating prepared by the present invention has high impact properties, and when buckles are 100cm, coating does not still occur slight crack completely.In burning initial stage foaming dense uniform, the later period forms a kind of bag-like Char Residues Structure that fire insulation is heat-insulated, and fire protecting performance is good.Preparation process flow is simple, convenient for operation.The fireproof coating belongs to water paint scope, belongs to green environmental friendly coatings, which can be widely used for timber structure.
Description
Technical field
The present invention relates to a kind of preparation of fireproof coating, the two-component transparent fire-resisting paint of especially a kind of high impact properties
And preparation method thereof.
Background technique
Currently, historic building structure fire complex genesis, hidden danger is numerous, once generating, loss is serious, not only to area and
Country brings serious casualties and property losses, certainly will also will cause the destruction of history and culture.Even to this day, China is also
The house of large quantities of residents and villager are mainly one in many old foreign-style houses in wood, brick structure, many cities, such as Shanghai
A little wooden building materials, many modern times house ornamentations pursuits are pseudo-classic, the furniture of wooden structures all used, if not to these wooden structures
It takes necessary fire to prevent, huge loss certainly will be will cause.The flame-proof treatment method of timber can be summarized in two classes substantially: one
Class is infusion process (also referred to as inherent flame retardant method), and another kind of is coating (also known as anti-flaming dope method).The treatment process of infusion process is multiple
It is miscellaneous, it is at high cost, and also the flame retardant treatment for carrying out essence to these intrinsic wooden buildings of ancient building artifact and object less may be used
Capable, this just needs to consider the method for coating protection.Coating protection method is at low cost with its, it is easy to operate, on ground original appearance influence it is small,
Integrate fire-resisting protection and decoration double effects and favored, also therefore becomes the first choice of old architecture survey.
The current country is to the developing focus or film forming matter of transparent fire-resisting paint and the selection of fire retardant.Fire prevention is applied
For material, film forming matter is particularly significant, it not only directly determines the physicochemical property of coating, while can also imitate to the fire prevention of coating
Fruit has a direct impact.Country's matrix resin selected when studying and preparing transparent fire-resisting paint is typically all amino-type
Resin has a lot of other resins not had this is because amino resins is applied as film forming matter in transparent fire-resisting paint
Advantage: (1) have both film forming matter and gas source double effects.Amino resins acts not only as the matrix of coating, and contains
Nitrogen source abundant, it is possible to reduce the problem of coating transparency caused by additional fire proofing additive declines；(2) reaction mechanism is clear.Ammonia
Base resin is as acid catalysis gel-type resin, when preparing fireproof coating as film forming matter using it, the class of fire retardant and curing agent
After type is more clear, and various phosphoric acid ester substances is added in fireproof system as fire retardant, while solidification can be played
The effect of agent, and amino resins solidifies influence of the structure of the mechanism and catalyst that are crosslinked to curing reaction and has also been obtained
Systematic research, in addition, the Relationship Comparison between the structure of resin, the type of catalyst and condition of cure and coating performance is clear
It is clear, it is bigger that transparent fire-resisting paint feasibility is developed based on this.
Till now, there are very big breakthrough in foreign countries from the last century 60's in terms of the research of transparent fire-resisting paint, and
And their not single research transparent fire-resisting paints, but each based flame retardant of comprehensive exploitation will then by reasonably matching
Different fire retardants is applied in different matrixes, this research and development for allowing for fire retardant is particularly important, but due to major part
The film forming matter of fireproof coating is all polymer, and fire retardant is mostly small molecule compound, this to develop be provided simultaneously with it is good
Physicochemical properties well, good decorative performance, the transparent fire-resisting paint of excellent flame retardant property are very difficult.
Currently, either domestic or foreign countries tend to research and develop integrated intumescent in terms of the exploitation of fire proofing
Flame-retardant polymer can play catalysis simultaneously, become the research of transparent fire-resisting paint at the highly effective flame-retardant system of charcoal, foaming effect
Emphasis is thus not necessarily to additional fire proofing additive, to enough obtain the preferable transparency.In addition transparent finishing fire retardant paint is limited
One big factor of application is exactly that the flexibility of coating is too poor, is easy cracking shortly after coated in solidifying on substrate, slightly collides one
Under will crack, not persistently.The present invention introduces soft segment in fire retardant systems, to improve the flexibility of coating, to mention
Its high shock resistance.
Summary of the invention
The purpose of the present invention is to solve the deficiencies of existing transparent fire-resisting paint, provide a kind of with high impact-resistant
The preparation method of the two-component transparent fire-resisting paint of property.
The purpose of the present invention can be achieved through the following technical solutions:
1. two-component transparent fire-resisting paint of a kind of high impact properties and preparation method thereof, it is characterised in that specific steps are such as
Under:
(1) preparation grafting water-base epoxy phosphate
Epoxy resin is dissolved in suitable solvent, temperature is 60~80 DEG C, and suitable amine substance is then added, and is reacted
Then 5-24h removes solvent, obtain aqueous epoxy resins.Then the water-base epoxy resin for taking suitable phosphoric acid and previously preparing
And suitable polyethylene glycol is sufficiently stirred in container, is warming up to 100~140 DEG C, reacts 2-10h, what discharging was grafted
Water-base epoxy phosphate flame retardant.Wherein content shared by phosphoric acid is 50~60%, and water-base epoxy phosphate is 30~40%, poly- second
Glycol is 5~15%, total weight 100%；The dosage of solvent is the 200%~300% of total weight.
(2) preparation of water-compatible amino resin
Solid formaldehyde and distilled water are added in there-necked flask, adjust PH to 8~9 with alkali, stirring adds melamine
Amine, is heated to that solution is limpid, and a small amount of pentaerythrite and urea is added when having in reaction a period of time when whiteness generation, is added
Alcohol is etherified 3~7h as etherifying agent, a small amount of urea is added, then to absorb unreacted formaldehyde.End product vacuum distillation,
Obtain water-compatible amino resin.
(3) preparation of fireproof coating
Grafting water-base epoxy phosphate flame retardant prepared by step (1) is compounded into stirring with water-compatible amino resin, can be obtained
To the transparent fire-resisting paint of two-component；The mass ratio of the described grafting water-base epoxy phosphate and water-compatible amino resin be 4:1~
1:1。
2. two-component transparent fire-resisting paint and its preparation side of a kind of high impact properties according to claim 1
Method, which is characterized in that the water-compatible amino resin is aqueous hexamethylolmelamine formaldehyde resin, aqueous depressionization trimerization
Cyanamide formaldehyde resin or aqueous Lauxite are one such or several.
3. two-component transparent fire-resisting paint and its preparation side of a kind of high impact properties according to claim 1
Method, which is characterized in that the alcohols etherifying agent is that methanol, n-butanol, isopropanol are one such.
4. two-component transparent fire-resisting paint and its preparation side of a kind of high impact properties according to claim 1
Method, which is characterized in that the polyethylene glycol is that PEG200, PEG400, PEG600, PEG800 are one such or several.
5. two-component transparent fire-resisting paint and its preparation side of a kind of high impact properties according to claim 1
Method, which is characterized in that the solvent is that ethyl alcohol, tetrahydrofuran, acetone are one such or several.
6. two-component transparent fire-resisting paint and its preparation side of a kind of high impact properties according to claim 1
Method, which is characterized in that the amine substance is diethanol amine, triethanolamine, three ethyl alcohol tetramines one or more.
Advantages of the present invention:
The two-component transparent fire-resisting paint handle of preparation contains acid source required for intumescent system, charcoal source, gas source, therefore protects
Coating has been demonstrate,proved with excellent fire protecting performance.Polyethylene glycol is introduced in fire retardant systems, so that the shock resistance of coating is big
Width improves, and coating is made to have excellent finishing effect.
Specific embodiment
Example one:
(1) 50g epoxy resin being dissolved in the ethyl alcohol of 500ml, temperature is 60 DEG C, suitable diethanol amine is then added,
5h is reacted, ethyl alcohol is then removed, obtains aqueous epoxy resins.Then the water-base epoxy resin 40g for taking 50g phosphoric acid and previously preparing
And 10g polyethylene glycol 400 is sufficiently stirred in container, is warming up to 100 DEG C, reaction 2, discharge the water-base epoxy being grafted
Phosphate flame retardant.
(2) solid formaldehyde and distilled water are added in there-necked flask, adjust PH to 8~9 with alkali, stirring adds trimerization
Cyanamide, is heated to that solution is limpid, and a small amount of pentaerythrite and urea is added when having in reaction a period of time when whiteness generation, adds
Enter methanol as etherifying agent and be etherified 3h, a small amount of urea is added, then to absorb unreacted formaldehyde.End product decompression is steamed
It evaporates, obtains water-compatible amino resin.
(3) by the water-compatible amino resin of the methanol etherification of preparation and the water-base epoxy phosphate of grafting with the mass ratio of 2:1
It is uniformly mixed, stirs 30min, cleared naturally to the bubble in coating to get two-component transparent fire-resisting paint is arrived.
Example two:
(1) 50g epoxy resin is dissolved in the tetrahydrofuran of 500ml, temperature is 70 DEG C, and suitable three ethyl alcohol is then added
Amine reacts 4h, then removes tetrahydrofuran, obtain aqueous epoxy resins.Then the water-base epoxy for taking 55g phosphoric acid and previously preparing
Resin 35g and 5g Macrogol 600 is sufficiently stirred in container, is warming up to 120 DEG C, reacts 3h, and discharge the water being grafted
Property epoxy phosphate ester fire retardant.
(2) solid formaldehyde and distilled water are added in there-necked flask, adjust PH to 8~9 with alkali, stirring adds trimerization
Cyanamide, is heated to that solution is limpid, and a small amount of pentaerythrite and urea is added when having in reaction a period of time when whiteness generation, adds
Enter positive definite alcohol as etherifying agent and be etherified 4h, a small amount of urea is added, then to absorb unreacted formaldehyde.End product decompression is steamed
It evaporates, obtains water-compatible amino resin.
(3) the water-base epoxy phosphate of the water-compatible amino resin and grafting that are etherified the n-butanol of preparation is with the quality of 1:1
Than being uniformly mixed, 30min is stirred, is cleared naturally to the bubble in coating to get two-component transparent fire-resisting paint is arrived.
Example three:
(1) 50g epoxy resin is dissolved in the acetone of 500ml, temperature is 80 DEG C, and suitable three ethyl alcohol four is then added
Amine reacts 4h, then removes acetone, obtain aqueous epoxy resins.Then the water-base epoxy resin for taking 55g phosphoric acid and previously preparing
35g and 5g polyethylene glycol 200 is sufficiently stirred in container, is warming up to 120 DEG C, reacts 3h, and discharge the aqueous ring being grafted
Oxygen phosphate flame retardant.
(2) solid formaldehyde and distilled water are added in there-necked flask, adjust PH to 8~9 with alkali, stirring adds trimerization
Cyanamide, is heated to that solution is limpid, and a small amount of pentaerythrite and urea is added when having in reaction a period of time when whiteness generation, adds
Enter isopropanol as etherifying agent and be etherified 4h, a small amount of urea is added, then to absorb unreacted formaldehyde.End product decompression is steamed
It evaporates, obtains water-compatible amino resin.
(3) the water-base epoxy phosphate of the water-compatible amino resin and grafting that are etherified the n-butanol of preparation is with the quality of 3:1
Than being uniformly mixed, 30min is stirred, is cleared naturally to the bubble in coating to get two-component transparent fire-resisting paint is arrived.
Claims (6)
1. two-component transparent fire-resisting paint of a kind of high impact properties and preparation method thereof, it is characterised in that specific step is as follows:
(1) preparation grafting water-base epoxy phosphate
Epoxy resin is dissolved in suitable solvent, temperature is 60~80 DEG C, and suitable amine substance is then added, and reacts 5-
For 24 hours, solvent is then removed, aqueous epoxy resins are obtained.Then take suitable phosphoric acid and the water-base epoxy resin that previously prepares with
And suitable polyethylene glycol is sufficiently stirred in container, is warming up to 100~140 DEG C, reacts 2-10h, discharge the water being grafted
Property epoxy phosphate ester fire retardant.Wherein content shared by phosphoric acid is 50~60%, and water-base epoxy phosphate is 30~40%, poly- second two
Alcohol is 5~15%, total weight 100%；The dosage of solvent is the 200%~300% of total weight.
(2) preparation of water-compatible amino resin
Solid formaldehyde and distilled water are added in there-necked flask, adjust PH to 8~9 with alkali, stirring adds melamine, adds
Heat is limpid to solution, and a small amount of pentaerythrite and urea is added when having in reaction a period of time when whiteness generation, and alcohol is added and makees
It is etherified 3~7h for etherifying agent, a small amount of urea is added, then to absorb unreacted formaldehyde.End product vacuum distillation, obtains
Water-compatible amino resin.
(3) preparation of fireproof coating
Grafting water-base epoxy phosphate flame retardant prepared by step (1) is compounded into stirring with water-compatible amino resin, can be obtained double
The transparent fire-resisting paint of component；The mass ratio of the grafting water-base epoxy phosphate and water-compatible amino resin is 4:1~1:1.
2. a kind of two-component transparent fire-resisting paint and preparation method thereof of high impact properties according to claim 1,
It is characterized in that, the water-compatible amino resin is aqueous hexamethylolmelamine formaldehyde resin, aqueous depressionization melamine
Formaldehyde resin or aqueous Lauxite are one such or several.
3. a kind of two-component transparent fire-resisting paint and preparation method thereof of high impact properties according to claim 1,
It is characterized in that, the alcohols etherifying agent is that methanol, n-butanol, isopropanol are one such.
4. a kind of two-component transparent fire-resisting paint and preparation method thereof of high impact properties according to claim 1,
It is characterized in that, the polyethylene glycol is that PEG200, PEG400, PEG600, PEG800 are one such or several.
5. a kind of two-component transparent fire-resisting paint and preparation method thereof of high impact properties according to claim 1,
It is characterized in that, the solvent is that ethyl alcohol, tetrahydrofuran, acetone are one such or several.
6. a kind of two-component transparent fire-resisting paint and preparation method thereof of high impact properties according to claim 1,
It is characterized in that, the amine substance is diethanol amine, triethanolamine, three ethyl alcohol tetramines one or more.
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| CN201810831482.3A CN108948942A (en) | 2018-07-26 | 2018-07-26 | A kind of two-component transparent fire-resisting paint of high impact properties and preparation method thereof |
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| CN201810831482.3A CN108948942A (en) | 2018-07-26 | 2018-07-26 | A kind of two-component transparent fire-resisting paint of high impact properties and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971219A (en) * | 2019-02-20 | 2019-07-05 | 常州鼎众冷暖设备工程有限公司 | A kind of preparation method of inorganic sealing hole agent |
| CN112358588A (en) * | 2020-11-10 | 2021-02-12 | 三棵树(上海)新材料研究有限公司 | High-solid-content amino resin for synthetic coating and preparation method thereof |
-
2018
- 2018-07-26 CN CN201810831482.3A patent/CN108948942A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109971219A (en) * | 2019-02-20 | 2019-07-05 | 常州鼎众冷暖设备工程有限公司 | A kind of preparation method of inorganic sealing hole agent |
| CN112358588A (en) * | 2020-11-10 | 2021-02-12 | 三棵树(上海)新材料研究有限公司 | High-solid-content amino resin for synthetic coating and preparation method thereof |
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