CN107446386A - Good coating modified calcium carbonate of a kind of dispersed effect and preparation method thereof - Google Patents

Good coating modified calcium carbonate of a kind of dispersed effect and preparation method thereof Download PDF

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CN107446386A
CN107446386A CN201710708081.4A CN201710708081A CN107446386A CN 107446386 A CN107446386 A CN 107446386A CN 201710708081 A CN201710708081 A CN 201710708081A CN 107446386 A CN107446386 A CN 107446386A
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parts
calcium carbonate
modified calcium
good coating
dispersed effect
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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
    • 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
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • 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
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/19—Oil-absorption capacity, e.g. DBP values

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention discloses good coating modified calcium carbonate of a kind of dispersed effect and preparation method thereof, the coating 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 coating 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 and compatibility with high molecular polymer is good.

Description

Good coating modified calcium carbonate of a kind of dispersed effect and preparation method thereof
【Technical field】
The invention belongs to modified calcium carbonate preparing technical field, and in particular to a kind of good coating of dispersed effect is modified Calcium carbonate and preparation method thereof.
【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 a kind of good coating modified calcium carbonate of dispersed effect and its system Preparation Method, existing calcium carbonate surface is hydrophilic and oleophobic, specific surface energy is high, easily reunites between particle to solve, with high molecular polymer Compatibility it is very poor the problems such as.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of good coating modified calcium carbonate of dispersed effect, 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.
Preferably, the good coating modified calcium carbonate of described dispersed effect, in units of parts by weight, including following original Material：Calcium carbonate 144-163 parts, AESA 4.2-5.4 parts, lauroyl peroxide 0.3-0.4 parts, three hydroxyls Methylpropane three (3- aziridinyls propionic ester) 0.5-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 parts, Diethylenetriamine pentacarboxylic acid potassium 1-1.2 parts, conditioning agent 0.4-0.5 parts, diisooctyl phthalate 1.6-2 parts, hexenyl are double Stearmide 0.5-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.5-0.6 parts, N- ethyls - 5- methyl -2- (1- Methylethyls) hexamethylene formamide 0.7-0.8 parts, stabilizer 0.4-0.5 parts.
Preferably, the good coating modified calcium carbonate of described dispersed effect, in units of parts by weight, including following original Material：144 parts of calcium carbonate, 4.2 parts of AESA, 0.3 part of lauroyl peroxide, trimethylolpropane tris 0.5 part of (3- aziridinyls propionic ester), 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- (2'- hydroxyls -3', 5'- bis- Tertiary phenyl) 0.5 part of -5- chlorinations BTA, 0.7 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, stably 0.4 part of agent.
Preferably, the conditioning agent is esters of acrylic acid conditioning agent.
Preferably, the stabilizer is modified alta-mud heat stabilizer.
The present invention also provides a kind of preparation method of the good coating modified calcium carbonate of dispersed effect, including following step Suddenly：
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 good coating modified calcium carbonate of dispersed effect is made.
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 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, oil factor it is low and It is good with the compatibility of high molecular polymer；
(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, coating 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 good coating modified calcium carbonate of the dispersed effect, in units of parts by weight, including it is following Raw material：Calcium carbonate 124-163 parts, AESA 2.8-5.4 parts, lauroyl peroxide 0.2-0.4 parts, three Hydroxymethyl-propane three (3- aziridinyls propionic ester) 0.4-0.6 parts, stannous chloride 0.1-0.2 parts, vanadic anhydride 0.2-0.3 Part, diethylenetriamine 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, hexenyl bis-stearamides 0.3-0.6 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTAs 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 good coating modified calcium carbonate of described dispersed effect, 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 good coating modified calcium carbonate of dispersed effect is made.
Below by more specific embodiment, the present invention will be described.
Embodiment 1
A kind of good coating modified calcium carbonate of dispersed effect, 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, esters of acrylic acid adjust Save 0.4 part of agent, 1.6 parts of diisooctyl phthalate, 0.5 part of hexenyl bis-stearamides, the 2- (uncles of 2'- hydroxyls -3', 5'- bis- Phenyl) 0.5 part of -5- chlorinations BTA, 0.7 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modification it is swollen Moisten native 0.4 part of heat stabilizer.
The preparation method of the good coating modified calcium carbonate of described dispersed effect, 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 good coating modified calcium carbonate of dispersed effect is made.
Embodiment 2
A kind of good coating modified calcium carbonate of dispersed effect, in units of parts by weight, including following raw material：Calcium carbonate 125 parts, 3 parts of AESA, 0.2 part of lauroyl peroxide, trimethylolpropane tris (3- aziridinyls third Acid esters) 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 adjust Save 0.3 part of agent, 1.2 parts of diisooctyl phthalate, 0.3 part of hexenyl bis-stearamides, the 2- (uncles of 2'- hydroxyls -3', 5'- bis- Phenyl) 0.3 part of -5- chlorinations BTA, 0.5 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modification it is swollen Moisten native 0.3 part of heat stabilizer.
The preparation method of the good coating modified calcium carbonate of described dispersed effect, 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 good coating modified calcium carbonate of dispersed effect is made.
Embodiment 3
A kind of good coating modified calcium carbonate of dispersed effect, in units of parts by weight, including following raw material：Calcium carbonate 162 parts, 5.2 parts of AESA, 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 0.5 part of conditioning agent, 2 parts of diisooctyl phthalate, 0.6 part of hexenyl bis-stearamides, the 2- (uncles of 2'- hydroxyls -3', 5'- bis- Phenyl) 0.6 part of -5- chlorinations BTA, 0.8 part of N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene formamide, modification it is swollen Moisten native 0.5 part of heat stabilizer.
The preparation method of the good coating modified calcium carbonate of described dispersed effect, 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 good coating modified calcium carbonate of dispersed effect is made.
Comparative example 1
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the good coating of dispersed effect and be modified Lack AESA, lauroyl peroxide, trimethylolpropane tris (3- ethylene imines in the raw material of calcium carbonate Base 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 good coating of dispersed effect and be modified Lack AESA in the raw material of calcium carbonate.
Comparative example 3
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the good coating of dispersed effect and be modified Lack lauroyl peroxide in the raw material of calcium carbonate.
Comparative example 4
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the good coating of dispersed effect and be modified Lack trimethylolpropane tris (3- aziridinyls propionic ester) in the raw material of calcium carbonate.
Comparative example 5
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the good coating of dispersed effect and be modified Lack stannous chloride in the raw material of calcium carbonate.
Comparative example 6
It is essentially identical with the preparation technology of embodiment 1, have only the difference is that preparing the good coating of dispersed effect and be modified Lack vanadic anhydride in the raw material of calcium carbonate.
Comparative example 7
The good coating of dispersed effect is the unmodified calcium carbonate of 1500 mesh same as Example 3 with modified calcium carbonate.
The good coating modified calcium carbonate product index of the dispersed effect prepared by embodiment 1-3 and comparative example 1-7 As a result 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 and compatibility with high molecular polymer is good；
(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, coating 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. good coating modified calcium carbonate of dispersed effect, it is characterised in that in units of parts by weight, including following original Material：Calcium carbonate 124-163 parts, AESA 2.8-5.4 parts, lauroyl peroxide 0.2-0.4 parts, three hydroxyls Methylpropane three (3- aziridinyls 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 parts, 2- (bis- tertiary phenyl of 2'- hydroxyls -3', 5'-) -5- chlorination BTA 0.3-0.6 parts, N- second Base -5- methyl -2- (1- Methylethyls) hexamethylene formamide 0.5-0.8 parts, stabilizer 0.3-0.5 parts.
  2. 2. the good coating modified calcium carbonate of dispersed effect according to claim 1, it is characterised in that using parts by weight as Unit, including following raw material：Calcium carbonate 144-163 parts, AESA 4.2-5.4 parts, peroxidating bay Acyl 0.3-0.4 parts, trimethylolpropane tris (3- aziridinyls propionic ester) 0.5-0.6 parts, stannous chloride 0.1-0.2 parts, five oxygen Change two vanadium 0.2-0.3 parts, diethylenetriamine 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 BTAs 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 good coating modified calcium carbonate of dispersed effect according to claim 2, it is characterised in that using parts by weight as Unit, including following raw material：144 parts of calcium carbonate, 4.2 parts of AESA, 0.3 part of lauroyl peroxide, 0.5 part of trimethylolpropane tris (3- aziridinyls propionic ester), 0.1 part of stannous chloride, 0.2 part of vanadic anhydride, divinyl three 1 part of amine 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'-) 0.5 part of -5- chlorinations BTA, N- ethyl -5- methyl -2- (1- Methylethyls) hexamethylene 0.7 part of formamide, 0.4 part of stabilizer.
  4. 4. the good coating modified calcium carbonate of dispersed effect according to claim any one of 1-3, it is characterised in that institute It is esters of acrylic acid conditioning agent to state conditioning agent.
  5. 5. the good coating modified calcium carbonate of dispersed effect according to claim any one of 1-3, it is characterised in that institute It is modified alta-mud heat stabilizer to state stabilizer.
  6. A kind of 6. preparation side of the good coating modified calcium carbonate of dispersed effect according to claim any one of 1-5 Method, it is characterised in that comprise 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 good coating modified calcium carbonate of dispersed effect is made.
  7. 7. the preparation method of the good coating modified calcium carbonate of dispersed effect according to claim 6, it is characterised in that Dried described in step S1 to water content≤0.4%.
  8. 8. the preparation method of the good coating modified calcium carbonate of dispersed effect according to claim 6, it is characterised in that The temperature being warming up to described in step S2 is 72-80 DEG C.
  9. 9. the preparation method of the good coating modified calcium carbonate of dispersed effect according to claim 6, it is characterised in that It is 75-85 DEG C that temperature is controlled described in step S3.
  10. 10. the preparation method of the good coating modified calcium carbonate of dispersed effect according to claim 6, its feature exist In it is 45-55 DEG C that temperature is controlled described in step S4.
CN201710708081.4A 2017-08-17 2017-08-17 Good coating modified calcium carbonate of a kind of dispersed effect and preparation method thereof Pending CN107446386A (en)

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CN106519775A (en) * 2016-09-29 2017-03-22 贺州钟山县双文碳酸钙新材料有限公司 Modified calcium carbonate for coating

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CN106082295A (en) * 2016-06-08 2016-11-09 江西广源化工有限责任公司 A kind of monolayer pyrophillite modified superfine ground calcium carbonate and preparation method thereof
CN106397838A (en) * 2016-09-29 2017-02-15 贺州钟山县双文碳酸钙新材料有限公司 Modified calcium carbonate for cables
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