CN108165083A - A kind of preparation method of aqueous alkide resin drier - Google Patents

A kind of preparation method of aqueous alkide resin drier Download PDF

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Publication number
CN108165083A
CN108165083A CN201711245598.0A CN201711245598A CN108165083A CN 108165083 A CN108165083 A CN 108165083A CN 201711245598 A CN201711245598 A CN 201711245598A CN 108165083 A CN108165083 A CN 108165083A
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solution
drier
alkide resin
aqueous alkide
isooctyl acid
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CN201711245598.0A
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谢新昇
王文新
史玉玲
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谢新昇
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D167/00Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
    • C09D167/08Polyesters modified with higher fatty oils or their acids, or with natural resins or resin acids

Abstract

The present invention relates to a kind of preparation methods of aqueous alkide resin drier, belong to technical field of fine.The present invention is with vanadium trichloride, basic zirconium chloride, cerium chloride, isooctyl acid is primary raw material, aqueous alkide resin drier is prepared for using organic acid saponification method, the present invention using isooctyl acid cerium as influence paint film surface drying main drier, it arranges in pairs or groups again zirconium iso-octoate and vanadium iso-octoate, it is very excellent to promote surface drying effect, after coating, which coats, to form a film, alkyd resin is gradually oxidized to peroxide, the metal ion strong with reproducibility reacts, form strong redox couple, bioactive molecule free radical is accelerated to be formed, and then promote alkyd resin rapid curing, due to film surface layer oxygen content height, alkyd resin is fast by oxidation rate, the amount of peroxides of formation is more, therefore surface layer cures faster, surface drying time is shorter.

Description

A kind of preparation method of aqueous alkide resin drier
Technical field
The present invention relates to a kind of preparation methods of aqueous alkide resin drier, belong to technical field of fine.
Background technology
In recent years, with the continuous improvement of people's environmental consciousness, the demand of water paint is continuously increased.With other resins It comparing, the advantage of aqueous alkide resin is to use a large amount of vegetable oil or aliphatic acid, smaller to oil product dependence, with The mode of air oxygen cures, so that resin solidification cost is relatively low, and it greatly reduces content, and having complied with environmental protection will It asks, therefore wide market.But a large amount of water exists, and changes the drying property of the resin.Therefore a kind of auxiliary agent is needed It improves the performance of aqueous alkide resin, and directly solvent type drier is introduced into aqueous alkide resin, there is very big office It is sex-limited.
Suitable complexing agent is added in conventional-type organometallic soap drier, increasing drier with this, reducing to lose dry is So far a kind of more effective method being widely used.Common complexing agent is mostly containing n-donor ligand, and organic ligand is in coating It is commonly referred to as the accelerating agent of drier.The addition of this kind of accelerating agent can be complexed with part metals ion in system, so as to reduce The loss of metal ion improves " losing dry " phenomenon in coating, accelerates the rate of drying of film.In addition, complexing agent The spin multiplicity for also affecting metal electron distribution is added in, and the presence of organic ligand produces relatively low energy track Antibonding orbital can promote the transfer of electronics, so as to which active drier be made to be maintained in the price of more living group.Although these accelerating agents Be effectively increased the activity of organic metal soap drier, but can not change drier itself color depth, viscosity is big, smell is heavy, The defects of toxicity is big, and the accelerating agent of nitrogenous class complexing agent can also further deepen the color of film in original degree.This The price of outer nitrogenous complexing agent is very high, and drier cost is caused to be substantially improved, is promoted the use of so as to also limit it.
Therefore in order to comply with the development trend of current aqueous alkide resin, exploitation is a kind of to be suitable for aqueous alkide resin system Drier be very necessary.
Invention content
The technical problems to be solved by the invention:For drier itself itself color depth, viscosity is big, smell is heavy, toxicity is big The problem of, provide a kind of preparation method of aqueous alkide resin drier.
In order to solve the above technical problems, the technical solution adopted by the present invention is:
A kind of preparation method of aqueous alkide resin drier, the specific steps are:
(1)Soybean oil, retinal 20~30min of heating stirring are taken, obtains solvent naphtha;
(2)Isooctyl acid is taken to add in solvent naphtha to be uniformly mixed, then sodium hydroxide solution is added dropwise, 70~80 are heated to after being added dropwise DEG C 3~5h of insulated and stirred, stratification simultaneously remove lower aqueous layer, then adjust pH to 6.5~7.5 with isooctyl acid, obtain saponified oil;
(3)Vanadium trichloride solution, zirconium oxychloride solution, solution of cerium chloride by oxidation is added dropwise successively into saponified oil, is kept the temperature after being added dropwise 3~5h is stirred, stratification simultaneously removes lower aqueous layer, obtains reaction solution;
(4)Reaction solution with deionized water is mixed and is cleaned by ultrasonic 10~20min, stratification simultaneously removes lower aqueous layer, repeats Anhydrous calcium chloride, anhydrous cupric sulfate are added in after cleaning 2~3 times, 1~2h of insulated and stirred, is cooled to room temperature at 70~80 DEG C Aqueous alkide resin drier.
Step(1)The mass ratio of the soybean oil and retinal is 1:1~3:1.
Step(1)The heating stirring process to be heated to 70~90 DEG C, with 300~400r/min insulated and stirreds 20~ 30min。
Step(2)The mass ratio of the isooctyl acid and solvent naphtha is 1:2~1:6.
Step(2)The mass fraction of the sodium hydroxide solution is 15%, and dosage is 0.6~2.4 times of isooctyl acid quality.
Step(3)The vanadium trichloride solution, zirconium oxychloride solution, solution of cerium chloride by oxidation are 60~120 parts by weight quality point Number is 10% vanadium trichloride solution, and 100~200 parts by weight mass fractions are 10% zirconium oxychloride solution, 90~180 parts by weight quality Score is 10% solution of cerium chloride by oxidation, and the vanadium trichloride solution usage is 0.6~2.4 times of isooctyl acid quality.
Step(4)The anhydrous calcium chloride dosage is the 1~4% of isooctyl acid quality.
Step(4)The anhydrous cupric sulfate dosage is the 1~4% of isooctyl acid quality.
Compared with other methods, advantageous effects are the present invention:
(1)The present invention is prepared using vanadium trichloride, basic zirconium chloride, cerium chloride, isooctyl acid as primary raw material using organic acid saponification method Aqueous alkide resin drier, the present invention, as the main drier of influence paint film surface drying, then are arranged in pairs or groups using isooctyl acid cerium Zirconium iso-octoate and vanadium iso-octoate, rush surface drying effect is very excellent, and after coating, which coats, to form a film, alkyd resin is gradually oxidized to Peroxide, the metal ion strong with reproducibility react, and form strong redox couple, accelerate bioactive molecule free radical shape Into, and then promote alkyd resin rapid curing, due to film surface layer oxygen content height, alkyd resin is fast by oxidation rate, formation Amount of peroxides is more, therefore surface layer curing is faster, and surface drying time is shorter;
(2)It is assisted while the anhydrous calcium chloride and anhydrous cupric sulfate that the present invention adds are as dehydrating agent with isooctyl acid coordination generation Drier is done solid work, the precipitation of zirconium in water is reduced, and bottom can also be promoted to dry, improves rate of drying and bin stability;
(3)It is the raw materials used in the present invention lighter color, nontoxic, efficient, be added in coating, paint film property is good, make paint film hardness, The performances such as adhesive force, color and luster, water resistance have greatly improved, and can improve gloss and gloss retention, while the whiteness having had again, change Drier itself color depth, the defects of viscosity is big, smell is heavy, toxicity is big.
Specific embodiment
200~300g soybean oils are taken, 100~200g retinals are fitted into flask, are heated to 70~90 DEG C, with 300~ 400r/min 20~30min of insulated and stirred, are cooled to room temperature to obtain solvent naphtha, take 50~100g isooctyl acids, and it is molten to add in 200~300g In agent oil, 20~30min is stirred, then 60~120g mass fractions are added dropwise as 15% hydrogen using 1~2g/min with 300~400r/min Sodium hydroxide solution is heated to 70~80 DEG C, 3~5h of insulated and stirred after being added dropwise, stand 1~2h and be layered and remove lower water Layer, then pH to 6.5~7.5 is adjusted with isooctyl acid, saponified oil is obtained, 60~120g is added dropwise with 1~2mL/min successively into saponified oil Mass fraction be 10% vanadium trichloride solution, 100~200g mass fractions be 10% zirconium oxychloride solution, 90~180g mass fractions For 10% solution of cerium chloride by oxidation, rear 3~5h of insulated and stirred is added dropwise, stands 1~2h and is layered and removes lower aqueous layer, then with 500~ 800mL temperature is mixed for 80~90 DEG C of deionized waters, and 10~20min is cleaned with 100W ultrasonic echographies, stands 1~2 layering simultaneously Remove lower aqueous layer, after repeated washing 2~3 times mixed liquor, add 1~2g anhydrous calcium chlorides, 1~2g anhydrous cupric sulfates, 1~2h of insulated and stirred at 70~80 DEG C is cooled to room temperature to obtain aqueous alkide resin drier.
Example 1
200g soybean oils are taken, 100g retinals are fitted into flask, are heated to 70 DEG C, with 300r/min insulated and stirred 20min, cooling Solvent naphtha is obtained to room temperature, takes 50g isooctyl acids, is added in 200g solvent naphthas, 20min is stirred, then with 1g/min drops with 300r/min 60g mass fractions is added to be heated to 70 DEG C, insulated and stirred 3h after being added dropwise for 15% sodium hydroxide solution, 1h is stood and is layered and goes PH to 6.5 is adjusted except lower aqueous layer, then with isooctyl acid, saponified oil is obtained, 60g mass is added dropwise successively with 1mL/min into saponified oil Score is 10% vanadium trichloride solution, and 100g mass fractions are 10% zirconium oxychloride solution, and 90g mass fractions are molten for 10% cerium chloride Liquid, is added dropwise rear insulated and stirred 3h, stands 1h and be layered and remove lower aqueous layer, then with 500mL temperature is 80 DEG C of deionized waters Mixing cleans 10min with 100W ultrasonic echographies, stands 1 and is layered and simultaneously removes lower aqueous layer, after repeated washing 2 times mixed liquor, 1g anhydrous calcium chlorides, 1g anhydrous cupric sulfates are added, the insulated and stirred 1h at 70 DEG C is cooled to room temperature to obtain aqueous alkide resin use Drier.
Example 2
250g soybean oils are taken, 150g retinals are fitted into flask, are heated to 80 DEG C, with 350r/min insulated and stirred 25min, cooling Solvent naphtha is obtained to room temperature, takes 75g isooctyl acids, is added in 250g solvent naphthas, 25min is stirred, then with 1g/min drops with 350r/min 90g mass fractions is added to be heated to 75 DEG C, insulated and stirred 4h after being added dropwise for 15% sodium hydroxide solution, 2h is stood and is layered and goes PH to 7.0 is adjusted except lower aqueous layer, then with isooctyl acid, saponified oil is obtained, 90g mass is added dropwise successively with 1mL/min into saponified oil Score is 10% vanadium trichloride solution, and 150g mass fractions are 10% zirconium oxychloride solution, and 135g mass fractions are molten for 10% cerium chloride Liquid, is added dropwise rear insulated and stirred 4h, stands 1h and be layered and remove lower aqueous layer, then with 650mL temperature is 85 DEG C of deionized waters Mixing cleans 15min with 100W ultrasonic echographies, stands 1 and is layered and simultaneously removes lower aqueous layer, after repeated washing 3 times mixed liquor, 2g anhydrous calcium chlorides, 2g anhydrous cupric sulfates are added, the insulated and stirred 1h at 75 DEG C is cooled to room temperature to obtain aqueous alkide resin use Drier.
Example 3
300g soybean oils are taken, 200g retinals are fitted into flask, are heated to 90 DEG C, with 400r/min insulated and stirred 30min, cooling Solvent naphtha is obtained to room temperature, takes 100g isooctyl acids, is added in 300g solvent naphthas, 30min is stirred, then with 2g/min drops with 400r/min 120g mass fractions is added to be heated to 80 DEG C, insulated and stirred 5h after being added dropwise for 15% sodium hydroxide solution, stand 2h layerings simultaneously Lower aqueous layer is removed, then pH to 7.5 is adjusted with isooctyl acid, saponified oil is obtained, 120g matter is added dropwise successively with 2mL/min into saponified oil Amount score is 10% vanadium trichloride solution, and 200g mass fractions are 10% zirconium oxychloride solution, and 180g mass fractions are 10% cerium chloride Solution, is added dropwise rear insulated and stirred 5h, stands 2h and be layered and remove lower aqueous layer, then with 800mL temperature is 90 DEG C of deionizations Water mixes, and 20min is cleaned with 100W ultrasonic echographies, stands 2 and is layered and simultaneously removes lower aqueous layer, must be mixed after repeated washing 3 times Liquid, adds 2g anhydrous calcium chlorides, 2g anhydrous cupric sulfates, and the insulated and stirred 2h at 80 DEG C is cooled to room temperature to obtain water alcohol acid tree Fat drier.
Aqueous alkide resin drier prepared by the present invention and the drier of Guangzhou company production are detected, and are had Body testing result such as following table table 1:
Table 1 aqueous alkide resin drier performance characterization
Aqueous alkide resin drier surface drying time that as shown in Table 1 prepared by the present invention does solid work that the time is short, water-tolerant, carries High rate of drying and bin stability using raw material lighter color, nontoxic, efficient, are added in coating, and paint film property is good, The performances such as hardness, adhesive force, color and luster, the water resistance of paint film have greatly improved, improve drier itself color depth, viscosity it is big, The defects of smell is heavy, toxicity is big has good application prospect.

Claims (8)

1. a kind of preparation method of aqueous alkide resin drier, which is characterized in that the specific steps are:
(1)Soybean oil, retinal 20~30min of heating stirring are taken, obtains solvent naphtha;
(2)Isooctyl acid is taken to add in solvent naphtha to be uniformly mixed, then sodium hydroxide solution is added dropwise, 70~80 are heated to after being added dropwise DEG C 3~5h of insulated and stirred, stratification simultaneously remove lower aqueous layer, then adjust pH to 6.5~7.5 with isooctyl acid, obtain saponified oil;
(3)Vanadium trichloride solution, zirconium oxychloride solution, solution of cerium chloride by oxidation is added dropwise successively into saponified oil, is kept the temperature after being added dropwise 3~5h is stirred, stratification simultaneously removes lower aqueous layer, obtains reaction solution;
(4)Reaction solution with deionized water is mixed and is cleaned by ultrasonic 10~20min, stratification simultaneously removes lower aqueous layer, repeats Anhydrous calcium chloride, anhydrous cupric sulfate are added in after cleaning 2~3 times, 1~2h of insulated and stirred, is cooled to room temperature at 70~80 DEG C Aqueous alkide resin drier.
A kind of 2. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(1) The mass ratio of the soybean oil and retinal is 1:1~3:1.
A kind of 3. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(1) The heating stirring process is is heated to 70~90 DEG C, with 300~400r/min insulated and stirreds, 20~30min.
A kind of 4. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(2) The mass ratio of the isooctyl acid and solvent naphtha is 1:2~1:6.
A kind of 5. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(2) The mass fraction of the sodium hydroxide solution is 15%, and dosage is 0.6~2.4 times of isooctyl acid quality.
A kind of 6. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(3) The vanadium trichloride solution, zirconium oxychloride solution, solution of cerium chloride by oxidation are that 60~120 parts by weight mass fractions are 10% vanadium trichloride Solution, 100~200 parts by weight mass fractions are 10% zirconium oxychloride solution, and 90~180 parts by weight mass fractions are 10% cerium chloride Solution, the vanadium trichloride solution usage are 0.6~2.4 times of isooctyl acid quality.
A kind of 7. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(4) The anhydrous calcium chloride dosage is the 1~4% of isooctyl acid quality.
A kind of 8. preparation method of aqueous alkide resin drier as described in claim 1, which is characterized in that step(4) The anhydrous cupric sulfate dosage is the 1~4% of isooctyl acid quality.
CN201711245598.0A 2017-12-01 2017-12-01 A kind of preparation method of aqueous alkide resin drier Pending CN108165083A (en)

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Publication number Priority date Publication date Assignee Title
CN110003707A (en) * 2019-03-11 2019-07-12 常州武城服饰有限公司 A kind of alkyd resin drier
CN110105874A (en) * 2019-05-09 2019-08-09 北京华东乐器有限公司 A kind of violin oil paint and its methods for making and using same

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CN101633819A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Preparation method of high efficient rare-earth paint drier
CN106634616A (en) * 2016-12-06 2017-05-10 广西科技大学 Preparation method of composite rare earth drier for oil paint

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CN101633819A (en) * 2008-07-23 2010-01-27 甘肃稀土新材料股份有限公司 Preparation method of high efficient rare-earth paint drier
CN106634616A (en) * 2016-12-06 2017-05-10 广西科技大学 Preparation method of composite rare earth drier for oil paint

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110003707A (en) * 2019-03-11 2019-07-12 常州武城服饰有限公司 A kind of alkyd resin drier
CN110105874A (en) * 2019-05-09 2019-08-09 北京华东乐器有限公司 A kind of violin oil paint and its methods for making and using same

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