CN107446385A - A kind of low modified calcium carbonate of oil factor and its application in paint - Google Patents

A kind of low modified calcium carbonate of oil factor and its application in paint Download PDF

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CN107446385A
CN107446385A CN201710707462.0A CN201710707462A CN107446385A CN 107446385 A CN107446385 A CN 107446385A CN 201710707462 A CN201710707462 A CN 201710707462A CN 107446385 A CN107446385 A CN 107446385A
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parts
calcium carbonate
modified calcium
oil factor
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梁胜仁
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Guangxi Huizhi Productivity Promotion Center Co Ltd
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Guangxi Huizhi Productivity Promotion Center Co Ltd
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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
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/021—Calcium carbonates
    • C09C1/022—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10—Treatment with macromolecular organic compounds
    • 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
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00

Abstract

The invention discloses a kind of low modified calcium carbonate of oil factor and its application in paint, the paint modified calcium carbonate, including following raw material：Calcium carbonate, AESA, lauroyl peroxide, trimethylolpropane tris (3 aziridinyl propionic ester), stannous chloride, vanadic anhydride, diethylenetriamine pentacarboxylic acid potassium, conditioning agent, diisooctyl phthalate, hexenyl bis-stearamides, 2 (2' hydroxyls 3', bis- tertiary phenyl of 5') 5 chlorination BTAs, N ethyls 5 methyl 2 (1 Methylethyl) hexamethylene formamide, stabilizer, the paint is by made of surface modification, property regulation, crushing, drying and other steps with modified calcium carbonate.The activation rate of the modified calcium carbonate of the present invention is high, and oil factor is low, good with other raw material components compatibilities applied in paint.

Description

A kind of low modified calcium carbonate of oil factor and its application in paint
【Technical field】
The invention belongs to modified calcium carbonate preparing technical field, and in particular to a kind of low modified calcium carbonate of oil factor and its Application in paint.
【Background technology】
Calcium carbonate is a kind of conventional inorganic filler, because source is wide, cheap etc., be widely used in plastics, rubber, coating, The fields such as stone slab, paint.But calcium carbonate surface is hydrophilic and oleophobic, specific surface energy is high, easily reunites between particle, with high molecular polymerization The compatibility of thing is very poor.Therefore, when being filled into high molecular polymer, it is necessary to calcium carbonate surface is modified, makes its table Face oleophilic drainage, enhancing and the compatibility of high molecular polymer, improve the dispersiveness in high molecular polymer, improve performance.
【The content of the invention】
The technical problem to be solved in the present invention is to provide low modified calcium carbonate of a kind of oil factor and preparation method thereof, with solution Certainly existing calcium carbonate surface is hydrophilic and oleophobic, specific surface energy is high, easily reunites between particle, very poor with the compatibility of high molecular polymer The problems such as.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of low modified calcium carbonate of oil factor, in units of parts by weight, including following raw material：Calcium carbonate 124-163 parts, AESA 2.8-5.4 parts, lauroyl peroxide 0.2-0.4 parts, trimethylolpropane tris (3- ethylene imines Base propionic ester) 0.4-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 parts, diethylenetriamine pentacarboxylic acid potassium 0.8-1.2 parts, conditioning agent 0.3-0.5 parts, diisooctyl phthalate 1.2-2 parts, hexenyl bis-stearamides 0.3-0.6 Part, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.3-0.6 parts, N- ethyl -5- methyl -2- (1- methyl Ethyl) hexamethylene formamide 0.5-0.8 parts, stabilizer 0.3-0.5 parts；
The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
S1：Calcium carbonate is crushed, crosses the sieve of 1200-1600 mesh, and is dried at being 85-90 DEG C in temperature, carbonic acid is made Calcium powder minces；
S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds aliphatic alcohol polyethenoxy Ether ammonium sulfate, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, rise Temperature, with 1000-1500r/min speed high-speed stirred 35-55min, mixture A is made；
S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, neighbour will be added in mixture A made from step S2 The isodecyl ester of phthalic acid two, hexenyl bis-stearamides, temperature is controlled, with 1000-1200r/min speed high-speed stirred 28- 36min, mixture B is made；
S4：2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations benzo three will be added in mixture B made from step S3 Azoles, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, temperature is controlled, with 800- 1000r/min speed high-speed stirred 18-32min, mixture C is made；
S5：Mixture C made from step S4 is crushed, crosses the sieve of 1200-1600 mesh, and in the case where temperature is 48-52 DEG C Dry to water content≤0.4%, the low modified calcium carbonate of oil factor is made.
Preferably, the low modified calcium carbonate of described oil factor, in units of parts by weight, including following raw material：Calcium carbonate 144-163 parts, AESA 4.2-5.4 parts, lauroyl peroxide 0.3-0.4 parts, trimethylolpropane Three (3- aziridinyls propionic ester) 0.5-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 parts, divinyl three Amine pentacarboxylic acid potassium 1-1.2 parts, conditioning agent 0.4-0.5 parts, diisooctyl phthalate 1.6-2 parts, hexenyl bis-stearamides 0.5-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.5-0.6 parts, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide 0.7-0.8 parts, stabilizer 0.4-0.5 parts.
Preferably, the low modified calcium carbonate of described oil factor, in units of parts by weight, including following raw material：Calcium carbonate 144 parts, 4.2 parts of AESA, 0.3 part of lauroyl peroxide, trimethylolpropane tris (3- aziridinyls Propionic ester) 0.5 part, 0.1 part of stannous chloride, 0.2 part of vanadic anhydride, 1 part of diethylenetriamine pentacarboxylic acid potassium, 0.4 part of conditioning agent, 1.6 parts of diisooctyl phthalate, 0.5 part of hexenyl bis-stearamides, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorine Change 0.5 part of BTA, 0.7 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, 0.4 part of stabilizer.
Preferably, the conditioning agent is esters of acrylic acid conditioning agent.
Preferably, the stabilizer is modified alta-mud heat stabilizer.
Preferably, dried described in step S1 to water content≤0.4%
Preferably, the temperature being warming up to described in step S2 is 72-80 DEG C.
Preferably, it is 75-85 DEG C that temperature is controlled described in step S3.
Preferably, it is 45-55 DEG C that temperature is controlled described in step S4.
The present invention also provides a kind of application of the low modified calcium carbonate of oil factor in paint, the paint using parts by weight as Unit, including following raw material：The low modified calcium carbonate 14-23 parts of rosin phenolic resin 45-68 parts, oil factor, cellulose acetate 7-13 parts, limonene 30-42 parts, 2,3- dimercapto -1- propyl alcohol 6-12 parts, phthalic anhydride 6-12 parts, two Benzalkonium 1- 2.5 parts, kh560 type silane coupler 0.6-2 parts.
The invention has the advantages that：
(1) from embodiment 1-3 and the data of comparative example 7, the activation rate of modified calcium carbonate is high, and oil factor is low, It is good with other raw material components compatibilities applied in paint；
(2) from embodiment 3 and comparative example 1-6 data, AESA, peroxidating bay Acyl, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride serve association in calcium carbonate modified Same-action, activation rate height and contact angle are improved, it is low to reduce oil factor；This is probably that table is used in calcium carbonate surface modifying Face modifying agent AESA, in conjunction with initiator lauroyl peroxide, crosslinking agent trimethylolpropane tris (3- aziridinyls propionic ester), accelerator stannous chloride and catalyst vanadic anhydride, significantly improve modified calcium carbonate Activation rate height, contact angle, oil factor are low, improve the compatibility with high molecular polymer；
(3) it is fatty with surface modifier is not added with modified calcium carbonate preparing raw material from the data of comparative example 2, paint Alcohol polyoxyethylene ether ammonium sulfate is to calcium carbonate surface modifying, the activation rate height of calcium carbonate, contact angle, oil factor others four relatively Component (lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride) changes most Greatly, illustrate that AESA serves vital effect in whole modified technique.
【Embodiment】
For ease of more fully understanding the present invention, it is illustrated by following instance, these examples belong to the protection of the present invention Scope, but do not limit the scope of the invention.
In embodiment, the low modified calcium carbonate of the oil factor, in units of parts by weight, including following raw material：Carbonic acid Calcium 124-163 parts, AESA 2.8-5.4 parts, lauroyl peroxide 0.2-0.4 parts, trihydroxy methyl third Alkane three (3- aziridinyls propionic ester) 0.4-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 parts, divinyl Triamine pentacarboxylic acid potassium 0.8-1.2 parts, esters of acrylic acid conditioning agent 0.3-0.5 parts, diisooctyl phthalate 1.2-2 parts, oneself Alkenyl bis-stearamides 0.3-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.3-0.6 parts, N- Ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide 0.5-0.8 parts, modified alta-mud heat stabilizer 0.3-0.5 parts.
The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
S1：Calcium carbonate is crushed, cross 1200-1600 mesh sieve, and temperature be 85-90 DEG C at dry to water content≤ 0.4%, obtained Paris white minces；
S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds aliphatic alcohol polyethenoxy Ether ammonium sulfate, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, rise Temperature arrives 72-80 DEG C, and with 1000-1500r/min speed high-speed stirred 35-55min, mixture A is made；
S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, neighbour will be added in mixture A made from step S2 The isodecyl ester of phthalic acid two, hexenyl bis-stearamides, it is 75-85 DEG C to control temperature, high with 1000-1200r/min speed Speed stirring 28-36min, is made mixture B；
S4：2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations benzo three will be added in mixture B made from step S3 Azoles, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, it is 45-55 to control temperature DEG C, with 800-1000r/min speed high-speed stirred 18-32min, mixture C is made；
S5：Mixture C made from step S4 is crushed, crosses the sieve of 1200-1600 mesh, and in the case where temperature is 48-52 DEG C Dry to water content≤0.4%, the low modified calcium carbonate of oil factor is made.
Application of the low modified calcium carbonate of the oil factor in paint, it is described to paint in units of parts by weight, including with Lower raw material：The low modified calcium carbonate 14-23 parts of rosin phenolic resin 45-68 parts, oil factor, cellulose acetate 7-13 parts, lemon Alkene 30-42 parts, 2,3- dimercapto -1- propyl alcohol 6-12 parts, phthalic anhydride 6-12 parts, two Benzalkonium 1-2.5 parts, kh560 Type silane coupler 0.6-2 parts.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of low modified calcium carbonate of oil factor, in units of parts by weight, including following raw material：144 parts of calcium carbonate, fat 4.2 parts of alcohol polyoxyethylene ether ammonium sulfate, 0.3 part of lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester) 0.5 Part, 0.1 part of stannous chloride, 0.2 part of vanadic anhydride, 1 part of diethylenetriamine pentacarboxylic acid potassium, 0.4 part of esters of acrylic acid conditioning agent, 1.6 parts of diisooctyl phthalate, 0.5 part of hexenyl bis-stearamides, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorine Change 0.5 part of BTA, 0.7 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud thermostabilization 0.4 part of agent.
The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
S1：Calcium carbonate is crushed, crosses the sieve of 1400 mesh, and it is 0.4% to be dried at being 88 DEG C in temperature to water content, system Paris white is obtained to mince；
S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds aliphatic alcohol polyethenoxy Ether ammonium sulfate, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, rise To 76 DEG C, with 1300r/min speed high-speed stirred 45min, mixture A is made in temperature；
S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, neighbour will be added in mixture A made from step S2 The isodecyl ester of phthalic acid two, hexenyl bis-stearamides, it is 80 DEG C to control temperature, with 1100r/min speed high-speed stirred 32min, mixture B is made；
S4：2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations benzo three will be added in mixture B made from step S3 Azoles, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, it is 50 DEG C to control temperature, With 900r/min speed high-speed stirred 25min, mixture C is made；
S5：Mixture C made from step S4 is crushed, crosses the sieve of 1400 mesh, and dried at being 50 DEG C in temperature to containing Water is 0.4%, and the low modified calcium carbonate of oil factor is made.
Application of the low modified calcium carbonate of the oil factor in paint, it is described to paint in units of parts by weight, including with Lower raw material：20 parts low of modified calcium carbonate of 54 parts of rosin phenolic resin, oil factor, 10 parts of cellulose acetate, 36 parts of limonene, 2, 9 parts of 3- dimercapto -1- propyl alcohol, 10 parts of phthalic anhydride, 1.8 parts of two Benzalkonium, 1.5 parts of kh560 types silane coupler.
Embodiment 2
A kind of low modified calcium carbonate of oil factor, in units of parts by weight, including following raw material：125 parts of calcium carbonate, fat 3 parts of alcohol polyoxyethylene ether ammonium sulfate, 0.2 part of lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester) 0.4 Part, 0.1 part of stannous chloride, 0.2 part of vanadic anhydride, 0.8 part of diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent 0.3 Part, 1.2 parts of diisooctyl phthalate, 0.3 part of hexenyl bis-stearamides, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) - 0.3 part of 5- chlorinations BTA, 0.5 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat 0.3 part of stabilizer.
The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
S1：Calcium carbonate is crushed, crosses the sieve of 1200 mesh, and it is 0.3% to be dried at being 85 DEG C in temperature to water content, system Paris white is obtained to mince；
S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds aliphatic alcohol polyethenoxy Ether ammonium sulfate, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, rise To 72 DEG C, with 1000r/min speed high-speed stirred 55min, mixture A is made in temperature；
S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, neighbour will be added in mixture A made from step S2 The isodecyl ester of phthalic acid two, hexenyl bis-stearamides, it is 75 DEG C to control temperature, with 1000r/min speed high-speed stirred 36min, mixture B is made；
S4：2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations benzo three will be added in mixture B made from step S3 Azoles, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, it is 45 DEG C to control temperature, With 800r/min speed high-speed stirred 32min, mixture C is made；
S5：Mixture C made from step S4 is crushed, crosses the sieve of 1200 mesh, and dried at being 48 DEG C in temperature to containing Water is 0.4%, and the low modified calcium carbonate of oil factor is made.
Application of the low modified calcium carbonate of the oil factor in paint, it is described to paint in units of parts by weight, including with Lower raw material：14 parts low of modified calcium carbonate of 45 parts of rosin phenolic resin, oil factor, 7 parts of cellulose acetate, 30 parts of limonene, 2, 6 parts of 3- dimercapto -1- propyl alcohol, 7 parts of phthalic anhydride, 1 part of two Benzalkonium, 0.8 part of kh560 types silane coupler.
Embodiment 3
A kind of low modified calcium carbonate of oil factor, in units of parts by weight, including following raw material：162 parts of calcium carbonate, fat 5.2 parts of alcohol polyoxyethylene ether ammonium sulfate, 0.4 part of lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester) 0.6 Part, 0.2 part of stannous chloride, 0.3 part of vanadic anhydride, 1.2 parts of diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent 0.5 Part, 2 parts of diisooctyl phthalate, 0.6 part of hexenyl bis-stearamides, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- 0.6 part of chlorination BTA, 0.8 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat are steady Determine 0.5 part of agent.
The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
S1：Calcium carbonate is crushed, crosses the sieve of 1500 mesh, and it is 0.4% to be dried at being 90 DEG C in temperature to water content, system Paris white is obtained to mince；
S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds aliphatic alcohol polyethenoxy Ether ammonium sulfate, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, rise To 80 DEG C, with 1500r/min speed high-speed stirred 35min, mixture A is made in temperature；
S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, neighbour will be added in mixture A made from step S2 The isodecyl ester of phthalic acid two, hexenyl bis-stearamides, it is 85 DEG C to control temperature, with 1200r/min speed high-speed stirred 28min, mixture B is made；
S4：2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations benzo three will be added in mixture B made from step S3 Azoles, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, it is 55 DEG C to control temperature, With 1000r/min speed high-speed stirred 18min, mixture C is made；
S5：Mixture C made from step S4 is crushed, crosses the sieve of 1600 mesh, and dried at being 52 DEG C in temperature to containing Water is 0.3%, and the low modified calcium carbonate of oil factor is made.
Application of the low modified calcium carbonate of the oil factor in paint, it is described to paint in units of parts by weight, including with Lower raw material：23 parts low of modified calcium carbonate of rosin phenolic resin 45-68 parts, oil factor, 13 parts of cellulose acetate, limonene 42 Part, 12 parts of 2,3- dimercapto -1- propyl alcohol, 12 parts of phthalic anhydride, 2.5 parts of two Benzalkonium, kh560 types silane coupler 2 Part.
Comparative example 1
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack in material AESA, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), Stannous chloride, vanadic anhydride.
Comparative example 2
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack AESA in material.
Comparative example 3
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack lauroyl peroxide in material.
Comparative example 4
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack trimethylolpropane tris (3- aziridinyls propionic ester) in material.
Comparative example 5
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack stannous chloride in material.
Comparative example 6
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the original of the low modified calcium carbonate of oil factor Lack vanadic anhydride in material.
Comparative example 7
The low modified calcium carbonate of oil factor is the unmodified calcium carbonate of 1500 mesh same as Example 3.
The low modified calcium carbonate product index result of the oil factor prepared by embodiment 1-3 and comparative example 1-7 see the table below.
Experimental project Oil factor (g/100g) Contact angle (°) Activation rate (%)
Embodiment 1 14.56 159.71 98.89
Embodiment 2 15.05 156.42 95.74
Embodiment 3 13.78 162.31 99.68
Comparative example 1 35.42 97.54 62.16
Comparative example 2 20.72 143.12 88.31
Comparative example 3 18.18 148.67 91.42
Comparative example 4 16.02 153.41 95.31
Comparative example 5 15.78 152.12 94.08
Comparative example 6 16.12 154.36 95.12
Comparative example 7 39.03 0 0
As seen from the above table：(1) from embodiment 1-3 and the data of comparative example 7, the activation rate of modified calcium carbonate Height, oil factor is low, good with other raw material components compatibilities applied in paint；
(2) from embodiment 3 and comparative example 1-6 data, AESA, peroxidating bay Acyl, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride serve association in calcium carbonate modified Same-action, activation rate height and contact angle are improved, it is low to reduce oil factor；This is probably that table is used in calcium carbonate surface modifying Face modifying agent AESA, in conjunction with initiator lauroyl peroxide, crosslinking agent trimethylolpropane tris (3- aziridinyls propionic ester), accelerator stannous chloride and catalyst vanadic anhydride, significantly improve modified calcium carbonate Activation rate height, contact angle, oil factor are low, improve the compatibility with high molecular polymer；
(3) it is fatty with surface modifier is not added with modified calcium carbonate preparing raw material from the data of comparative example 2, paint Alcohol polyoxyethylene ether ammonium sulfate is to calcium carbonate surface modifying, the activation rate height of calcium carbonate, contact angle, oil factor others four relatively Component (lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride) changes most Greatly, illustrate that AESA serves vital effect in whole modified technique.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, for the skill of this area For art personnel, the present invention can have various modifications and variations.Within the spirit and principles of the invention, that is made any repaiies Change, equivalent substitution, improvement etc., should be included in the scope of the protection.

Claims (10)

  1. A kind of 1. low modified calcium carbonate of oil factor, it is characterised in that in units of parts by weight, including following raw material：Calcium carbonate 124-163 parts, AESA 2.8-5.4 parts, lauroyl peroxide 0.2-0.4 parts, trimethylolpropane Three (3- aziridinyls propionic ester) 0.4-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 parts, divinyl three Amine pentacarboxylic acid potassium 0.8-1.2 parts, conditioning agent 0.3-0.5 parts, diisooctyl phthalate 1.2-2 parts, hexenyl stearic bicine diester Amine 0.3-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.3-0.6 parts, N- ethyl -5- methyl - 2- (1- Methylethyls) hexamethylene formamide 0.5-0.8 parts, stabilizer 0.3-0.5 parts；
    The preparation method of the low modified calcium carbonate of described oil factor, comprises the following steps：
    S1：Calcium carbonate is crushed, crosses the sieve of 1200-1600 mesh, and is dried at being 85-90 DEG C in temperature, Paris white is made Mince；
    S2：Paris white made from step S1 is minced and is added in high-speed mixer, adds AEO sulphur Sour ammonium, lauroyl peroxide, trimethylolpropane tris (3- aziridinyls propionic ester), stannous chloride, vanadic anhydride, heating, With 1000-1500r/min speed high-speed stirred 35-55min, mixture A is made；
    S3：Diethylenetriamine pentacarboxylic acid potassium, esters of acrylic acid conditioning agent, adjacent benzene two will be added in mixture A made from step S2 The isodecyl ester of formic acid two, hexenyl bis-stearamides, temperature is controlled, with 1000-1200r/min speed high-speed stirred 28- 36min, mixture B is made；
    S4：Will in mixture B made from step S3 add 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorinations BTA, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modified alta-mud heat stabilizer, temperature is controlled, with 800- 1000r/min speed high-speed stirred 18-32min, mixture C is made；
    S5：Mixture C made from step S4 is crushed, crosses the sieve of 1200-1600 mesh, and dried at being 48-52 DEG C in temperature To water content≤0.4%, the low modified calcium carbonate of oil factor is made.
  2. 2. the low modified calcium carbonate of oil factor according to claim 1, it is characterised in that in units of parts by weight, including Following raw material：Calcium carbonate 144-163 parts, AESA 4.2-5.4 parts, lauroyl peroxide 0.3-0.4 Part, trimethylolpropane tris (3- aziridinyls propionic ester) 0.5-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2- 0.3 part, diethylenetriamine pentacarboxylic acid potassium 1-1.2 parts, conditioning agent 0.4-0.5 parts, diisooctyl phthalate 1.6-2 parts, oneself Alkenyl bis-stearamides 0.5-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.5-0.6 parts, N- Ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide 0.7-0.8 parts, stabilizer 0.4-0.5 parts.
  3. 3. the low modified calcium carbonate of oil factor according to claim 2, it is characterised in that in units of parts by weight, including Following raw material：144 parts of calcium carbonate, 4.2 parts of AESA, 0.3 part of lauroyl peroxide, trihydroxy methyl third 0.5 part of alkane three (3- aziridinyls propionic ester), 0.1 part of stannous chloride, 0.2 part of vanadic anhydride, diethylenetriamine pentacarboxylic acid potassium 1 Part, 0.4 part of conditioning agent, 1.6 parts of diisooctyl phthalate, 0.5 part of hexenyl bis-stearamides, 2- (2'- hydroxyl -3', Bis- tertiary phenyl of 5'-) 0.5 part of -5- chlorinations BTA, 0.7 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, 0.4 part of stabilizer.
  4. 4. the low modified calcium carbonate of oil factor according to claim any one of 1-3, it is characterised in that the conditioning agent is Esters of acrylic acid conditioning agent.
  5. 5. the low modified calcium carbonate of oil factor according to claim any one of 1-3, it is characterised in that the stabilizer is Modified alta-mud heat stabilizer.
  6. 6. the low modified calcium carbonate of oil factor according to claim 1, it is characterised in that dried described in step S1 to containing Water≤0.4%.
  7. 7. the low modified calcium carbonate of oil factor according to claim 1, it is characterised in that be warming up to described in step S2 Temperature is 72-80 DEG C.
  8. 8. the low modified calcium carbonate of oil factor according to claim 1, it is characterised in that control temperature described in step S3 For 75-85 DEG C.
  9. 9. the low modified calcium carbonate of oil factor according to claim 1, it is characterised in that control temperature described in step S4 For 45-55 DEG C.
  10. A kind of 10. application of the low modified calcium carbonate of oil factor according to claim 1 in paint, it is characterised in that The paint is in units of parts by weight, including following raw material：The low modified calcium carbonate of rosin phenolic resin 45-68 parts, oil factor 14-23 parts, cellulose acetate 7-13 parts, limonene 30-42 parts, 2,3- dimercapto -1- propyl alcohol 6-12 parts, phthalic anhydride 6- 12 parts, two Benzalkonium 1-2.5 parts, kh560 type silane coupler 0.6-2 parts.
CN201710707462.0A 2017-08-17 2017-08-17 A kind of low modified calcium carbonate of oil factor and its application in paint Pending CN107446385A (en)

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Application publication date: 20171208