CN116463002A - Friction gun auxiliary agent for powder coating and preparation method thereof - Google Patents
Friction gun auxiliary agent for powder coating and preparation method thereof Download PDFInfo
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- CN116463002A CN116463002A CN202211707933.5A CN202211707933A CN116463002A CN 116463002 A CN116463002 A CN 116463002A CN 202211707933 A CN202211707933 A CN 202211707933A CN 116463002 A CN116463002 A CN 116463002A
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- 239000000843 powder Substances 0.000 title claims abstract description 24
- 238000000576 coating method Methods 0.000 title claims abstract description 23
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 20
- 239000011248 coating agent Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000002253 acid Substances 0.000 claims abstract description 26
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 14
- 230000003078 antioxidant effect Effects 0.000 claims description 11
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 238000005070 sampling Methods 0.000 claims description 8
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 8
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 6
- YKGBNAGNNUEZQC-UHFFFAOYSA-N 6-methyl-n,n-bis(6-methylheptyl)heptan-1-amine Chemical compound CC(C)CCCCCN(CCCCCC(C)C)CCCCCC(C)C YKGBNAGNNUEZQC-UHFFFAOYSA-N 0.000 claims description 5
- BVFSYZFXJYAPQJ-UHFFFAOYSA-N butyl(oxo)tin Chemical compound CCCC[Sn]=O BVFSYZFXJYAPQJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000001530 fumaric acid Substances 0.000 claims description 5
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229920005862 polyol Polymers 0.000 claims description 4
- 150000003077 polyols Chemical class 0.000 claims description 4
- 150000007519 polyprotic acids Polymers 0.000 claims description 4
- -1 stearyl alcohol ester Chemical class 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- XTTGYFREQJCEML-UHFFFAOYSA-N tributyl phosphite Chemical compound CCCCOP(OCCCC)OCCCC XTTGYFREQJCEML-UHFFFAOYSA-N 0.000 claims description 4
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 3
- PXGZQGDTEZPERC-UHFFFAOYSA-N 1,4-cyclohexanedicarboxylic acid Chemical compound OC(=O)C1CCC(C(O)=O)CC1 PXGZQGDTEZPERC-UHFFFAOYSA-N 0.000 claims description 3
- PISLZQACAJMAIO-UHFFFAOYSA-N 2,4-diethyl-6-methylbenzene-1,3-diamine Chemical compound CCC1=CC(C)=C(N)C(CC)=C1N PISLZQACAJMAIO-UHFFFAOYSA-N 0.000 claims description 3
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 claims description 3
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 3
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 3
- DSKYSDCYIODJPC-UHFFFAOYSA-N 2-butyl-2-ethylpropane-1,3-diol Chemical compound CCCCC(CC)(CO)CO DSKYSDCYIODJPC-UHFFFAOYSA-N 0.000 claims description 2
- SAIKULLUBZKPDA-UHFFFAOYSA-N Bis(2-ethylhexyl) amine Chemical compound CCCCC(CC)CNCC(CC)CCCC SAIKULLUBZKPDA-UHFFFAOYSA-N 0.000 claims description 2
- OPKOKAMJFNKNAS-UHFFFAOYSA-N N-methylethanolamine Chemical compound CNCCO OPKOKAMJFNKNAS-UHFFFAOYSA-N 0.000 claims description 2
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 claims description 2
- 239000001361 adipic acid Substances 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- LUZSPGQEISANPO-UHFFFAOYSA-N butyltin Chemical compound CCCC[Sn] LUZSPGQEISANPO-UHFFFAOYSA-N 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- GOQYKNQRPGWPLP-UHFFFAOYSA-N n-heptadecyl alcohol Natural products CCCCCCCCCCCCCCCCCO GOQYKNQRPGWPLP-UHFFFAOYSA-N 0.000 claims description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 2
- 150000003014 phosphoric acid esters Chemical class 0.000 claims description 2
- 238000006068 polycondensation reaction Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000376 reactant Substances 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 claims 1
- 150000005846 sugar alcohols Polymers 0.000 claims 1
- 230000009477 glass transition Effects 0.000 abstract description 7
- 229920001225 polyester resin Polymers 0.000 abstract description 4
- 239000004645 polyester resin Substances 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 description 8
- 238000005886 esterification reaction Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229920000728 polyester Polymers 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000007590 electrostatic spraying Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- 229940035437 1,3-propanediol Drugs 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- FAOSYNUKPVJLNZ-UHFFFAOYSA-N butylstannane Chemical compound CCCC[SnH3] FAOSYNUKPVJLNZ-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/20—Polyesters having been prepared in the presence of compounds having one reactive group or more than two reactive groups
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/52—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation
- C08G63/54—Polycarboxylic acids or polyhydroxy compounds in which at least one of the two components contains aliphatic unsaturation the acids or hydroxy compounds containing carbocyclic rings
-
- 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
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
- Paints Or Removers (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The invention provides a friction gun auxiliary agent for powder coating and a preparation method thereof. The acid value of the synthesized polyester resin is less than 5mg KOH/g, the hydroxyl value is 20-70mg KOH/g, the viscosity is 3000-10000cps@200 ℃, and the glass transition temperature is 50-70 ℃. When the powder coating prepared by adding the auxiliary agent into the powder coating resin is sprayed by using a friction gun, the resin has high chargeability, and the sprayed part has uniform powder coating, good leveling property and excellent surface property.
Description
Technical Field
The invention belongs to the field of coatings, and particularly relates to a friction gun auxiliary agent for powder coatings and a preparation method thereof.
Background
The common spraying processes of powder paint are electrostatic spraying and friction gun spraying. Electrostatic spraying has been widely used in the market, and has the advantages of lower requirements for powder coating, thus being capable of meeting the use requirements of most resins, but also having the major defects that dead angles appear when complex workpieces are sprayed, and powder is difficult to be applied to part of corners. At present, the electrostatic spray gun manufacturer is optimized, the occurrence probability of dead angle phenomenon is smaller and smaller, but the dead angle phenomenon still cannot be avoided. In contrast, friction gun spraying can well solve the problem of dead angles of complex workpieces, but also has higher requirements on the chargeability of powder coatings.
Because the electrostatic spraying process cannot meet the requirements of thick workpieces of customers in the current market, I specially develop a friction gun auxiliary agent suitable for powder coating. After the auxiliary agent is used for powder preparation, the friction gun is used for spraying, the resin has good charging performance, a thick workpiece can be completely covered, no dead angle appears, the surface performance and the impact performance are excellent, the requirements of customers are met, and along with the market development and the increase of the variety of the workpiece, the polyester resin for the friction gun has wider prospect.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a UV light curing primer with high solid content and capable of improving the coating adhesive force, and a preparation method and a use method thereof.
The invention aims at realizing the following technical scheme:
the polyester resin for the friction gun comprises the following raw materials in parts by weight:
the friction gun auxiliary agent for the powder coating provided by the invention is prepared by the following steps:
1) The first stage: adding the polyol, the polybasic acid and the catalyst which are weighed according to the proportion into a reaction kettle, introducing nitrogen into the reaction kettle, gradually heating to 220-240 ℃, reacting for 6-9 hours until the reactant is clear and transparent, testing the acid value to be less than 15mgKOH/g, the hydroxyl value to be 30-90mgKOH/g, and the viscosity to be 500-2500cps@200 ℃;
2) And a second stage: cooling to 200-220 ℃, vacuumizing by a vacuum pump to perform polycondensation reaction, vacuumizing for 0.5-2 hours under the vacuum degree of-0.098 to-0.1 Mpa, sampling to be clear and transparent, and testing the acid value to be less than 5mgKOH/g, the hydroxyl value to be 20-70mgKOH/g and the viscosity to be 3000-10000cps@200 ℃;
3) And a third stage: adding a certain amount of auxiliary agent and antioxidant, cooling to 190-210 ℃ and discharging.
Preferably, the polyol in step 1) comprises a diol and a triol; wherein the dihydric alcohol is selected from one or more of neopentyl glycol, 2-butyl-2-ethyl-1, 3-propylene glycol, 1, 4-cyclohexanedimethanol, ethylene glycol, diethylene glycol, 1, 4-butanediol and 1, 6-hexanediol, and the trihydric alcohol is trimethylolpropane or glycerol.
Preferably, the polyacid in step 1) comprises one or more of terephthalic acid, isophthalic acid, 1, 4-cyclohexanedicarboxylic acid, fumaric acid, adipic acid.
Preferably, the catalyst in the step 1) is one of monobutyl tin oxide, n-butyl tin trioctoate and stannous oxalate.
Preferably, in the step 3), the auxiliary agent is an organic amine, including one or more of triethylamine, tri-N-butylamine, triisooctylamine, diisooctylamine, diethyltoluenediamine, N' -bis (2-hydroxyethyl) ethylenediamine, N-diisopropylethylenediamine and N-methyl-2-hydroxyethylamine, and the auxiliary agent is used for friction charging with a friction rod and a pipe wall material in a friction gun when the powder resin is sprayed on the friction gun, so that the coating is uniformly distributed on the surface of a thick workpiece.
Preferably, the antioxidant in the step 3) is one or more of various phosphate esters, including tributyl phosphite, phenyl phosphite, stearyl alcohol ester and lauryl alcohol ester, and mainly plays a role in antioxidation.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a friction gun auxiliary agent for powder coating and a preparation method thereof. The acid value of the synthesized polyester resin is less than 5mgKOH/g, the hydroxyl value is 20-70mgKOH/g, the viscosity is 3000-10000cps@200 ℃, and the glass transition temperature is 50-70 ℃. When the powder coating prepared by adding the auxiliary agent into the powder coating resin is sprayed by using a friction gun, the resin has high chargeability, and the sprayed part has uniform powder coating, good leveling property and excellent surface property.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The first step: 400 parts by mass of neopentyl glycol, 7 parts by mass of trimethylolpropane, 21 parts by mass of ethylene glycol, 650 parts by mass of terephthalic acid, 16 parts by mass of hexamethylene dicarboxylic acid and 1 part by mass of a catalyst (monobutyl tin oxide) are added into a reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to about 240 ℃ at a rate of 20 ℃/40min, the reaction is carried out for 8 hours, the sample is taken, the resin is colorless and transparent, the acid value, the hydroxyl value and the viscosity of the resin are measured, and water generated by the esterification reaction is collected.
And a second step of: when the acid value reaches 12mgKOH/g and the hydroxyl value reaches 40mgKOH/g, the viscosity is 1100cps@200 ℃, the temperature is controlled to 220 ℃, the reaction kettle is vacuumized for 1h, the vacuum degree is-0.098 to-0.1 Mpa, and sampling is carried out after the vacuum is finished to determine the acid value, the hydroxyl value and the viscosity.
And a third step of: when the acid value reaches 1mgKOH/g, the hydroxyl value is 30mgKOH/g, the viscosity is 600 cps@200 ℃, the temperature is reduced to 210 ℃, 50 parts by mass of tri-n-butylamine and 10 parts by mass of triphenyl phosphite serving as an antioxidant are added, and the mixture is stirred for 20 minutes and discharged. The glass transition temperature of the polyester is 64 ℃.
Example 2
The first step: 410 parts by mass of neopentyl glycol, 20 parts by mass of trimethylolpropane, 22 parts by mass of 1, 3-propanediol and 666 parts by mass of terephthalic acid and 1 part by mass of a catalyst (monobutyl tin oxide) are added into a reaction kettle, nitrogen is introduced into the reaction kettle, the temperature is raised to about 240 ℃ at a rate of 20 ℃/40min, the reaction is carried out for 8 hours, the sample is taken, the resin is colorless and transparent, the acid value, the hydroxyl value and the viscosity of the resin are measured, and water generated by the esterification reaction is collected.
And a second step of: when the acid value reaches 11mgKOH/g and the hydroxyl value reaches 55mgKOH/g, the viscosity is 1500cps@200 ℃, the temperature is controlled to 220 ℃, the reaction kettle is vacuumized for 1h, the vacuum degree is minus 0.098 to minus 0.1Mpa, and the acid value, the hydroxyl value and the viscosity are measured by sampling after the vacuum is finished.
And a third step of: when the acid value reaches 1mgKOH/g, the hydroxyl value reaches 42mgKOH/g, the viscosity is at 8000cps@200 ℃, the temperature is reduced to 210 ℃, 45 parts by mass of triisooctyl amine and 10 parts by mass of antioxidant triphenyl phosphite are added, and the mixture is stirred for 20 minutes and discharged. The glass transition temperature of the polyester is 66 ℃.
Example 3
The first step: to the reaction vessel, 413 parts by mass of neopentyl glycol, 6 parts by mass of trimethylolpropane, 35 parts by mass of 1, 4-cyclohexanedimethanol, 618 parts by mass of terephthalic acid, 50 parts by mass of fumaric acid and 0.6 part by mass of a catalyst (n-butyltin trioctoate) were added, and nitrogen was introduced into the reaction vessel, and the reaction vessel was heated to about 240℃at a rate of 20℃per 40 minutes, reacted for 8.5 hours, sampled, and the resin was colorless and transparent, and the acid value, hydroxyl value and viscosity of the resin were measured, and water produced by the esterification reaction was collected.
And a second step of: when the acid value reaches 11mgKOH/g and the hydroxyl value reaches 45mgKOH/g, the viscosity is 1200cps@200 ℃, the temperature is controlled to 220 ℃, the reaction kettle is vacuumized for 0.7h, the vacuum degree is minus 0.098 to minus 0.1Mpa, and the acid value, the hydroxyl value and the viscosity are measured by sampling after the vacuum is finished.
And a third step of: when the acid value reaches 2mgKOH/g, the hydroxyl value reaches 34mgKOH/g, the viscosity is 4500cps@200 ℃, the temperature is reduced to 210 ℃, 45 parts by mass of triisooctyl amine and 8 parts by mass of tributyl phosphite serving as an antioxidant are added, and the mixture is stirred for 20 minutes and discharged. The glass transition temperature of the polyester is 60 ℃.
Example 4
The first step: to the reaction vessel, 413 parts by mass of neopentyl glycol, 8 parts by mass of trimethylolpropane, 40 parts by mass of 1, 4-butanediol, 650 parts by mass of terephthalic acid, 10 parts by mass of 1, 4-cyclohexanedicarboxylic acid, 40 parts by mass of fumaric acid and 1 part by mass of a catalyst (monobutyltin oxide) were added, nitrogen was introduced into the reaction vessel, the temperature was raised to about 240℃at a rate of 20℃per 40min, the reaction was carried out for 8 hours, sampling was carried out, the resin was colorless and transparent, the acid value, hydroxyl value and viscosity of the resin were measured, and water produced by the esterification reaction was collected.
And a second step of: when the acid value reaches 9.5mgKOH/g and the hydroxyl value reaches 50mgKOH/g, the viscosity is 1100cps@200 ℃, the temperature is controlled to 220 ℃, the reaction kettle is vacuumized for 1.5 hours, the vacuum degree is-0.098 to-0.1 Mpa, and sampling is carried out after the vacuum is finished to determine the acid value, the hydroxyl value and the viscosity.
And a third step of: when the acid value reaches 0.6mgKOH/g, the hydroxyl value reaches 38mgKOH/g, the viscosity reaches 5500cps@200 ℃, the temperature is reduced to 210 ℃, 40 parts by mass of diethyl toluenediamine and 8 parts by mass of tributyl phosphite serving as an antioxidant are added, and the mixture is stirred for 20 minutes and discharged. The glass transition temperature of the polyester is 62 ℃.
Example 5
The first step: 400 parts by mass of neopentyl glycol, 30 parts by mass of trimethylolpropane, 40 parts by mass of 1, 6-hexanediol, 500 parts by mass of terephthalic acid, 180 parts by mass of isophthalic acid, 20 parts by mass of fumaric acid and 1.2 parts by mass of a catalyst (stannous oxalate) are added into a reaction kettle, nitrogen is introduced into the reaction kettle, the reaction is carried out at a rate of 20 ℃/40min to about 240 ℃ for 8 hours, the sample is taken, the resin is colorless and transparent, the acid value, the hydroxyl value and the viscosity of the resin are measured, and water generated by the esterification reaction is collected.
And a second step of: when the acid value reaches 8mgKOH/g, the hydroxyl value is 66mgKOH/g, the viscosity is 1800cps@200deg.C, the temperature is controlled to 220 ℃, the reaction kettle is vacuumized for 1h, the vacuum degree is-0.098 to-0.1 Mpa, and the acid value, the hydroxyl value and the viscosity are measured by sampling after the vacuum is finished.
And a third step of: when the acid value reaches 0.5mgKOH/g, the hydroxyl value reaches 55mgKOH/g, the viscosity is 8900cps@200 ℃, the temperature is reduced to 210 ℃, 45 parts by mass of triisooctyl amine and 10 parts by mass of antioxidant triphenyl phosphite are added, and the mixture is stirred for 20 minutes and discharged. The glass transition temperature of the polyester is 56 ℃.
A commercially available W resin was used as a base resin, 5% of the friction gun auxiliary agent synthesized in each example was added, and the base performance was tested after spraying with a friction gun without adding the comparative example, as shown in the following Table:
the performance test shows that when the auxiliary agent is added into the powder coating prepared from the powder coating resin, and the friction gun is used for spraying, the resin has high chargeability, so that the sample plate has good leveling performance and excellent surface performance. Meets the requirement of thick workpiece spraying, realizes no dead angle of spraying
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (7)
1. The friction gun auxiliary agent for the powder coating is characterized by comprising the following raw materials in parts by weight:
35-45 parts of polyalcohol
50-60 parts of polybasic acid
0.01 to 0.1 part of catalyst
2-5 parts of auxiliary agent
0.1-1 part of antioxidant.
2. A method of preparing a friction gun adjuvant for powder coatings according to claim 1, said method comprising the steps of:
1) The first stage: adding the polyol, the polybasic acid and the catalyst which are weighed according to the proportion into a reaction kettle, introducing nitrogen into the reaction kettle, gradually heating to 220-240 ℃, reacting for 6-9 hours until the reactant is clear and transparent, testing the acid value to be less than 15mgKOH/g, the hydroxyl value to be 30-90mgKOH/g, and the viscosity to be 500-2500cps@200 ℃;
2) And a second stage: cooling to 200-220 ℃, vacuumizing by a vacuum pump to perform polycondensation reaction, vacuumizing for 0.5-2 hours under the vacuum degree of-0.098 to-0.1 Mpa, sampling to be clear and transparent, and testing the acid value to be less than 5mgKOH/g, the hydroxyl value to be 20-70mgKOH/g and the viscosity to be 3000-10000cps@200 ℃;
3) And a third stage: adding a certain amount of auxiliary agent and antioxidant, cooling to 190-210 ℃ and discharging.
3. The method of claim 2, wherein the polyol in step 1) comprises a diol and a triol; wherein the dihydric alcohol is selected from one or more of neopentyl glycol, 2-butyl-2-ethyl-1, 3-propylene glycol, 1, 4-cyclohexanedimethanol, ethylene glycol, diethylene glycol, 1, 4-butanediol and 1, 6-hexanediol, and the trihydric alcohol is trimethylolpropane or glycerol.
4. The method according to claim 2, wherein the polybasic acid in step 1) comprises one or more of terephthalic acid, isophthalic acid, 1, 4-cyclohexanedicarboxylic acid, fumaric acid, and adipic acid.
5. The preparation method according to claim 2, wherein the catalyst in the step 1) is one of monobutyl tin oxide, n-butyl tin trioctoate and stannous oxalate.
6. The preparation method of claim 2, wherein the auxiliary agent in the step 3) is an organic amine, including one or more of triethylamine, tri-N-butylamine, triisooctylamine, diisooctylamine, diethyltoluenediamine, N' -bis (2-hydroxyethyl) ethylenediamine, N-diisopropylethylenediamine and N-methyl-2-hydroxyethylamine, and the auxiliary agent is used for friction charging with friction rods and pipe wall materials in a friction gun when powder resin is sprayed by the friction gun, so that the coating is uniformly distributed on the surface of a thick workpiece.
7. The preparation method according to claim 2, wherein the antioxidant in the step 3) is one or more of various phosphate esters including tributyl phosphite, phenyl phosphite, stearyl alcohol ester and lauryl alcohol ester, and has an antioxidant effect.
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| US5021473A (en) * | 1987-11-05 | 1991-06-04 | Hoechst Aktiengesellschaft | Process for enhancing the electrostatic chargeability of powder coatings or powders, and the use thereof for surface-coating solid objects |
| CN103897101A (en) * | 2014-04-23 | 2014-07-02 | 郑州大学 | Acrylic polyester-type hyperdispersant and preparation method and application thereof |
| CN104277682A (en) * | 2014-10-31 | 2015-01-14 | 安徽神剑新材料股份有限公司 | Powder coating sprayed through friction gun |
| CN110373095A (en) * | 2019-07-05 | 2019-10-25 | 浙江聚华材料科技股份有限公司 | A kind of preparation method for the powdery paints improving powder utilization |
| CN112384548A (en) * | 2019-09-18 | 2021-02-19 | 擎天材料科技有限公司 | Polyester resin, preparation method thereof, powder coating and workpiece |
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2022
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5021473A (en) * | 1987-11-05 | 1991-06-04 | Hoechst Aktiengesellschaft | Process for enhancing the electrostatic chargeability of powder coatings or powders, and the use thereof for surface-coating solid objects |
| CN103897101A (en) * | 2014-04-23 | 2014-07-02 | 郑州大学 | Acrylic polyester-type hyperdispersant and preparation method and application thereof |
| CN104277682A (en) * | 2014-10-31 | 2015-01-14 | 安徽神剑新材料股份有限公司 | Powder coating sprayed through friction gun |
| CN110373095A (en) * | 2019-07-05 | 2019-10-25 | 浙江聚华材料科技股份有限公司 | A kind of preparation method for the powdery paints improving powder utilization |
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