CN104877199A - Method for preparing rubber masterbatch by calcium carbonate dispersed by lignin - Google Patents
Method for preparing rubber masterbatch by calcium carbonate dispersed by lignin Download PDFInfo
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- CN104877199A CN104877199A CN201510365962.1A CN201510365962A CN104877199A CN 104877199 A CN104877199 A CN 104877199A CN 201510365962 A CN201510365962 A CN 201510365962A CN 104877199 A CN104877199 A CN 104877199A
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- rubber
- calcium carbonate
- xylogen
- lignin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/06—Copolymers with styrene
Abstract
Provided is a method for preparing rubber masterbatch by calcium carbonate dispersed by lignin. The method comprises two working sections of lignin dispersed calcium carbonate filler preparing by the lignin dispersed calcium carbonate and blending of filter and rubber. In the first working section, water, the lignin and the calcium carbonate are mixed according to a certain proportion, then ball milling is performed on a ball mill to obtain paste of the lignin dispersed calcium carbonate, dehydration is performed on the obtained paste in a air drying oven of 60-70 DEG C or in a vacuum drying oven to enable the water content of the paste to be 10-30 percent, and then the lignin dispersed calcium carbonate filter is obtained. In the second working section, the calcium carbonate filter dispersed by the lignin in the first working section and rubber are blended through an open mill or an internal mixer, and then are prilled through a double-screw extruder to prepare rubber masterbatch materials. Application research shows that the rubber masterbatch materials can be used as a reinforcing agent to greatly improve the mechanical properties of rubber materials. The method has the advantages that the preparation technology is simple, raw materials are low in price and easy to obtain, and meanwhile the lignin belongs to a product of comprehensive utilization of resources.
Description
Technical field
The present invention relates to a kind of method that calcium carbonate utilizing xylogen to disperse prepares rubber master batches, belong to rubber filling modification and resources circulation field of comprehensive utilization.
Background technology
Inorganic nano-filler generally has the advantages such as rigidity, dimensional stability and thermostability, high molecular polymer has the advantages such as toughness, workability and electrical property as plastics, rubber, resin etc., but the shortcoming such as inorganic filler particle and macromolecular material polarity difference are large, difficulty is mixed into, difficulty is disperseed, directly affect the performance of polymer composite.By certain method, mineral filler is modified, change the polarity on inorganic filler particle surface, then itself and polymer are carried out compound, the consistency between inorganic filler surface and polymer materials can be improved, thus improve the performance of polymer composites.Calcium carbonate has a kind ofly industrially produced and in macromolecular material, obtained the filler of the cheapness of widespread use.When long time without surface modification, calcium carbonate is difficult to dispersed in the polymer, is thus difficult to produce modified effect to polymkeric substance.At present fatty alcohol, Aluminate, lipid acid, siloxanes etc. are mainly contained, as Chinese patent CN104497638A, CN104479415A, CN104497637A, CN1597531A etc. to the chemical surface modification agent of calcium carbonate.The calcium carbonate that fatty alcohol, Aluminate, lipid acid, siloxanes etc. are modified applies to the aspect such as plastics, rubber to be existed mechanical property and promotes the problems such as little and production cost is high.
Summary of the invention
Xylogen is the waste produced in pulping and papermaking processes.Its molecular structure belongs to space three-dimensional structure, has aromatic base, phenolic hydroxyl group, alcoholic extract hydroxyl group, carbonyl, methoxyl group, carboxyl, conjugated double bond isoreactivity group, thus gives xylogen better properties by chemical modification.Calcium carbonate is a kind of common mineral filler, comparatively extensive in field application such as rubber, plastics, coating, optics.The object of the invention is the shortcoming existed for existing Technlolgy of Surhce Modincation Of Calcium Carbonate, provide a kind of xylogen that utilizes and the method for disperse modified is carried out to calcium carbonate, and added rubber and prepare rubber master batches, apply to rubber materials, while improving the over-all properties of material, reduce production cost.
Technical scheme of the present invention is a kind of method that calcium carbonate utilizing xylogen to disperse prepares rubber master batches.Its concrete preparation method and processing step as follows:
(1) under room temperature condition, water, xylogen and calcium carbonate is blended to carry out wet ball grinding under the rotating speed of 250-400rpm on ball mill after mixing (wherein water be xylogen and calcium carbonate quality sum 60-80%) by certain proportioning, obtain the calcium carbonate slurry of xylogen dispersion.
(2) slurry obtained by (1) is positioned in the air dry oven of 60-70 DEG C or vacuum drying oven and dewaters, make slurry water content be 10-30%, obtain the pearl filler of xylogen dispersion.
(3) rubber is plasticated on a mill until to bag roller, add the pearl filler disperseed by the xylogen of preparation in (2) in proportion, mixing to constant weight at a certain temperature; Or the pearl filler in Banbury mixer, rubber and xylogen the disperseed blended calcium carbonate rubber master batch prepared rubber/xylogen and disperse at a certain temperature; Mixing rubber master batch is obtained rubber master batch material by double-screw extruding pelletizing.
The present invention by utilize xylogen disperse calcium carbonate, for the production of rubber filling master batch material, its advantage and positively effect as follows:
1, the calcium carbonate of xylogen dispersion, for the production of rubber filling masterbatch, good dispersity, and product surface is bright.
2, in the inventive method, xylogen is paper industry renewable resource, calcium carbonate abundance, and production technique is simple, and prepared filler can significantly improve the mechanical property of rubber, has good economic benefit.
specific embodiment mode
A kind of xylogen is utilized to disperse calcium carbonate to prepare the method for rubber master batches and rubber composite illustrates the present invention in further detail below in conjunction with specific embodiment and subordinate list to provided by the invention.
Specific embodiment 1: paracril/xylogen dispersion calcium carbonate composite material
(1) under room temperature condition, 600 grams of xylogen (being as the criterion with dry lignin quality) are mixed with the ratio (xylogen: calcium carbonate=3:2) of 400 grams of calcium carbonate (water-ground limestone 1500 order) in quality 3:2, and the water high speed machine adding 600 grams puts it in ball grinder after mixing 10 minutes, with wet ball grinding under the rotating speed of 350rpm 4 hours on ball mill, obtain the slurry of the pearl filler of xylogen dispersion.
(2) slurry obtained by (1) is put in the air dry oven of 70 DEG C to dewater, and makes its slurry water content be 20%, obtains the pearl filler of xylogen dispersion.
(3) paracril is plasticated on a mill until to bag roller, it is 100 parts by paracril number in mass fraction, the ratio of the pearl filler 300 parts of xylogen dispersion adds blended, melting temperature is 100 DEG C, mixing to constant weight, prepare paracril/xylogen dispersion calcium carbonate rubber master batch (100:300); Mixing rubber master batch is obtained paracril master batch material (paracril/xylogen dispersion calcium carbonate=100:300) by double-screw extruding pelletizing.
(4) by the formula consumption in table 1, first by paracril low-temperature plasticizing 10 minutes on a mill until, then paracril master batch material is added successively, BIPB, at room temperature mixing 20 minutes, thin-pass also played triangle bag 12 times, bottom sheet, prepares the calcium carbonate/paracril rubber unvulcanizate of xylogen dispersion.
Table 1 nitile-butadiene rubber composite material formula
| Component | Mass fraction |
| Paracril master batch material (corresponding amount of filler) | Variable (20,40,60,80) |
| Paracril (comprising glue amount in rubber master batch) | 100 |
| BIPB | 2.5 |
Glue stuff compounding is parked 24 hours, utilize vulcanizing press sulfuration, cure conditions is 170 DEG C/10MPa × T
90,obtain lignin-modified calcium carbonate/nitile-butadiene rubber composite material.
The calcium carbonate of xylogen of the present invention dispersion also it can be used as filler to be filled into testing method in rubber: the performance-vulcanization characteristics of cross-linked rubber, tensile strength, elongation, hardness are carried out according to standard GB/T/T 16584-1996, GB/T 528-1998, GB/T 531-1999, GB/T 3512-2001 respectively, and its mechanical property is in table 2.
The performance of table 2 xylogen dispersion calcium carbonate/nitile-butadiene rubber composite material
Comparative example 1: organic decoration water-ground limestone/nitile-butadiene rubber composite material
At room temperature, in mill to paracril carry out cold plastication add successively after 20 minutes organic decoration water-ground limestone (1500 order) and BIPB(formula in table 3) rubber ingredients, evenly mixing on a mill until, thin-pass 12 bottom sheet, use vulcanizing press sulfuration at 170 DEG C after rubber unvulcanizate being placed 24 h, its mechanical property is in table 4.
Table 3 paracril basic recipe
| Component | Massfraction |
| Paracril | 100 |
| BIPB | 2.5 |
Table 4 organic decoration water-ground limestone/nitile-butadiene rubber composite material mechanical property
Experimental result shows: the matrix material that paracril master batch material prepared by the present invention is prepared as paracril filler, and its performance is better than organic decoration calcium carbonate (1500 order)/nitile-butadiene rubber composite material.
Specific embodiment 2: the calcium carbonate composite material of styrene-butadiene rubber(SBR)/xylogen dispersion
(1) pearl filler of xylogen dispersion is prepared by preparation method in embodiment 1.
(2) styrene-butadiene rubber(SBR) is plasticated on a mill until to bag roller, it is 100 parts by styrene-butadiene rubber(SBR) number in mass fraction, the ratio of the pearl filler 300 parts of xylogen dispersion adds blended, melting temperature is 100 DEG C, mixing to constant weight, prepare styrene-butadiene rubber(SBR)/xylogen dispersion calcium carbonate rubber master batch (100:300); Mixing rubber master batch is obtained styrene-butadiene rubber(SBR) master batch material (styrene-butadiene rubber(SBR)/xylogen dispersion calcium carbonate=100:300) by double-screw extruding pelletizing.
(3) by the formula consumption in table 5, first by styrene-butadiene rubber(SBR) low-temperature plasticizing 10 minutes on a mill until, then styrene-butadiene rubber(SBR) master batch material is added successively, BIPB, at room temperature mixing 20 minutes, thin-pass also played triangle bag 12 times, bottom sheet, prepares xylogen dispersion calcium carbonate/styrene-butadiene rubber(SBR) rubber unvulcanizate.
Table 5 styrene-butadiene rubber composite material formula
| Component | Mass fraction |
| Styrene-butadiene rubber(SBR) master batch material (corresponding amount of filler) | Variable (20,40,60,80) |
| Styrene-butadiene rubber(SBR) (comprising glue amount in rubber master batch) | 100 |
| BIPB | 1.5 |
Glue stuff compounding is parked 24 hours, utilize vulcanizing press sulfuration, cure conditions is 160 DEG C/10MPa × T
90,obtain lignin-modified calcium carbonate/styrene-butadiene rubber composite material.
Xylogen of the present invention dispersion calcium carbonate also it can be used as filler to be filled into testing method in rubber: the performance-vulcanization characteristics of cross-linked rubber, tensile strength, elongation, hardness are carried out according to standard GB/T/T 16584-1996, GB/T 528-1998, GB/T 531-1999, GB/T 3512-2001 respectively, and its mechanical property is in table 6.
The performance of table 6 xylogen dispersion calcium carbonate/styrene-butadiene rubber composite material
Comparative example 2: organic decoration water-ground limestone/styrene-butadiene rubber composite material
At room temperature, add successively after styrene-butadiene rubber(SBR) being plasticated 15 minutes in mill organic decoration water-ground limestone (1500 order) and BIPB(formula in table 7) rubber ingredients, evenly mixing on a mill until, thin-pass 12 bottom sheet, use vulcanizing press sulfuration at 160 DEG C after rubber unvulcanizate being placed 24 h, its mechanical property is in table 8.
Table 7 styrene-butadiene rubber(SBR) basic recipe
| Component | Massfraction |
| Styrene-butadiene rubber(SBR) | 100 |
| BIPB | 1.5 |
Table 8 organic decoration water-ground limestone/styrene-butadiene rubber composite material mechanical property
Experimental result shows: the matrix material that styrene-butadiene rubber(SBR) master batch material prepared by the present invention is prepared as styrene-butadiene rubber(SBR) filler, and its performance is better than organic decoration water-ground limestone (1500 order)/nitile-butadiene rubber composite material.
Specific embodiment 3: cis-1,4-polybutadiene rubber/xylogen dispersion calcium carbonate composite material
(1) pearl filler of xylogen dispersion is prepared by preparation method in embodiment 1.
(2) cis-1,4-polybutadiene rubber is plasticated on a mill until to bag roller, it is 100 parts by cis-1,4-polybutadiene rubber number in mass fraction, the ratio of the pearl filler 300 parts of xylogen dispersion adds blended, melting temperature is 100 DEG C, mixing to constant weight, prepare cis-1,4-polybutadiene rubber/xylogen dispersion calcium carbonate rubber master batch (100:300); Mixing rubber master batch is obtained cis-1,4-polybutadiene rubber master batch material (cis-1,4-polybutadiene rubber/xylogen dispersion calcium carbonate=100:300) by Screw Extrusion granulation.
(3) by the formula consumption in table 9, first by cis-1,4-polybutadiene rubber low-temperature plasticizing 10 minutes on a mill until, then cis-1,4-polybutadiene rubber master batch material is added successively, BIPB, at room temperature mixing 20 minutes, thin-pass also played triangle bag 12 times, bottom sheet, prepares the calcium carbonate/cis-1,4-polybutadiene rubber rubber unvulcanizate of xylogen dispersion.
Table 9 cis-1,4-polybutadiene rubber composite-material formula
| Component | Mass fraction |
| Cis-1,4-polybutadiene rubber master batch material (corresponding amount of filler) | Variable (20,40,60,80) |
| Cis-1,4-polybutadiene rubber (comprising glue amount in rubber master batch) | 100 |
| BIPB | 1.0 |
Glue stuff compounding is parked 24 hours, utilize vulcanizing press sulfuration, cure conditions is 150 DEG C/10MPa × T
90,obtain xylogen dispersion calcium carbonate/cis-1,4-polybutadiene rubber matrix material.
The calcium carbonate of xylogen of the present invention dispersion also it can be used as filler to be filled into testing method in rubber: the performance-vulcanization characteristics of cross-linked rubber, tensile strength, elongation, hardness are carried out according to standard GB/T/T 16584-1996, GB/T 528-1998, GB/T 531-1999, GB/T 3512-2001 respectively, and its mechanical property is in table 10.
The performance of table 10 xylogen dispersion calcium carbonate/cis-1,4-polybutadiene rubber matrix material
Comparative example 3: organic decoration water-ground limestone/cis-1,4-polybutadiene rubber matrix material
At room temperature, add successively after cis-1,4-polybutadiene rubber being plasticated 5 minutes in mill organic decoration water-ground limestone (1500 order) and BIPB(formula in table 11) rubber ingredients, evenly mixing on a mill until, thin-pass 12 bottom sheet, use vulcanizing press sulfuration at 150 DEG C after rubber unvulcanizate being placed 24 h, its mechanical property is in table 12.
Table 11 cis-1,4-polybutadiene rubber basic recipe
| Component | Massfraction |
| Cis-1,4-polybutadiene rubber | 100 |
| BIPB | 1.0 |
Table 12 organic decoration water-ground limestone/cis-1,4-polybutadiene rubber composite materials property
Experimental result shows: cis-1,4-polybutadiene rubber master batch material prepared by the present invention is as cis-1,4-polybutadiene rubber filler, and its performance is better than organic decoration water-ground limestone (1500 order).The application test of the rubber master batch of the calcium carbonate content of other glue kinds and the dispersion of different xylogen is all under equal conditions better than commodity water-ground limestone, does not enumerate all cases as space is limited.
Claims (8)
1. the calcium carbonate utilizing xylogen to disperse prepares a method for rubber master batches, and its concrete preparation method comprises following processing step:
(1) under room temperature condition, blended to carry out ball milling under the rotating speed of 250-400rpm on ball mill after water, xylogen are mixed by certain proportioning with calcium carbonate, obtain the slurry of the calcium carbonate of xylogen dispersion;
(2) slurry obtained by (1) be positioned in the air dry oven of 60-70 DEG C or dewater in vacuum drying oven, making slurry water content be 10-30%, obtaining the pearl filler of xylogen dispersion;
(3) rubber is plasticated on a mill until to bag roller, add the pearl filler disperseed by the xylogen of preparation in (2) in proportion, mixing to constant weight at a certain temperature; Or the pearl filler in Banbury mixer, rubber and xylogen the disperseed blended calcium carbonate rubber master batch prepared rubber/xylogen and disperse at a certain temperature; Mixing rubber master batch is obtained rubber master batch material by double-screw extruding pelletizing.
2. prepare the method for rubber master batches according to a kind of calcium carbonate utilizing xylogen to disperse according to claim 1, it is characterized in that the method comprise the dispersion of xylogen to calcium carbonate prepare xylogen dispersion pearl filler and xylogen dispersion pearl filler and blend rubber granulation Liang Ge workshop section.
3. prepare the method for rubber master batches according to a kind of calcium carbonate utilizing xylogen to disperse according to claim 1, it is characterized in that xylogen can be anhydrous or contain a certain amount of water.
4. prepare the method for rubber master batches according to a kind of calcium carbonate utilizing xylogen to disperse according to claim 1, it is characterized in that the water content of filler is 10-30%.
5. prepare the method for rubber master batches according to a kind of calcium carbonate utilizing xylogen to disperse according to claim 1, it is characterized in that calcium carbonate is one or more mixing in water-ground limestone, light calcium carbonate, activated Calcium carbonate.
6. prepare the method for rubber master batches according to a kind of calcium carbonate utilizing xylogen to disperse according to claim 1, its feature controls at 60-120 at the melting temperature of mill or Banbury mixer
oc.
7. a kind of calcium carbonate utilizing xylogen to disperse prepares the method for rubber master batches according to claim 1, and in master batch material, the pearl filler proportion of xylogen dispersion is 1-95%.
8. a kind of calcium carbonate utilizing xylogen to disperse according to claim 1 prepares the method for rubber master batches, its application of rubber kind comprises: paracril, styrene-butadiene rubber(SBR), cis-1,4-polybutadiene rubber, natural rubber, chlorinatedpolyethylene, ethylene propylene rubber, terpolymer EP rubber, epichlorohydrin rubber, wherein one or more such as chloroprene rubber.
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Cited By (5)
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| CN106883472A (en) * | 2017-04-26 | 2017-06-23 | 国网河南方城县供电公司 | A kind of transformer sealing ring elastomeric material and preparation method thereof |
| CN107383460A (en) * | 2017-09-25 | 2017-11-24 | 安徽依采妮纤维材料科技有限公司 | A kind of preparation method of the compound modified rubber material of lignin calcium carbonate |
| CN107936330A (en) * | 2017-12-13 | 2018-04-20 | 马鞍山市荣亿密封材料有限责任公司 | A kind of preparation method of salt tolerant modified butadiene acrylonitrile rubber polyurethane resin vulcanizate sealing material |
| CN115851209A (en) * | 2022-12-08 | 2023-03-28 | 浙江多邦新材料有限公司 | Polyurethane hot melt adhesive for composite fabric and preparation method thereof |
| WO2024045226A1 (en) * | 2022-08-31 | 2024-03-07 | 三维控股集团股份有限公司 | Graphene-modified chloroprene rubber and high-performance rubber v belt prepared from same |
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Application publication date: 20150902 |